Syntheses and Characterization of Palladium Complexes with a Hemilabile “PCO” Pincer Ligand
Fulmer, Gregory R.; Kaminsky, Werner; Kemp, Richard A.; Goldberg, Karen I.; Organometallics 30 (2011) 1627–; doi:10.1021/om101150y

data_4064140
_publ_section_title
;
 Syntheses and Characterization of Palladium Complexes with a Hemilabile
 &#x201C;PCO&#x201D; Pincer Ligand
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1627
_journal_paper_doi               10.1021/om101150y
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C18 H29 O4 P Pd, 1.5(C6 D6)'
_chemical_formula_sum            'C27 H29 D9 O4 P Pd'
_chemical_formula_weight         573
_chemical_name_common            (tBuPCO)PdO(CO)OH
_chemical_name_systematic        (8)
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 94.3110(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6066(2)
_cell_length_b                   10.5079(2)
_cell_length_c                   25.9114(5)
_cell_measurement_reflns_used    350
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     2608.23(9)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_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  0.0252
_diffrn_reflns_av_unetI/netI     0.0154
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            70254
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         33.19
_diffrn_reflns_theta_min         1.58
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.803
_exptl_absorpt_correction_T_max  0.8959
_exptl_absorpt_correction_T_min  0.7947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.473
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         9975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0204
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0177P)^2^+1.4083P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0499
_reflns_number_gt                9216
_reflns_number_total             9975
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om101150y_si_002.cif
_cod_data_source_block           (8)
_cod_database_code               4064140