Synthesis and Reactivity of Mixed-Ligand Palladium(II) Organometallic Complexes with Phosphites and Bis(pyrazol-1-yl)methane
Bortoluzzi, Marco; Paolucci, Gino; Pitteri, Bruno; Vavasori, Andrea; Bertolasi, Valerio; Organometallics 28 (2009) 3247–; doi:10.1021/om900146a

data_4069341
_publ_section_title
;
 Synthesis and Reactivity of Mixed-Ligand Palladium(II) Organometallic
 Complexes with Phosphites and Bis(pyrazol-1-yl)methane
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              3247
_journal_paper_doi               10.1021/om900146a
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C14 H26 N4 O3 P Pd, Cl O4'
_chemical_formula_sum            'C14 H26 Cl N4 O7 P Pd'
_chemical_formula_weight         535.21
_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                 96.5022(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.6637(2)
_cell_length_b                   9.5738(2)
_cell_length_c                   19.8507(4)
_cell_measurement_reflns_used    15228
_cell_measurement_temperature    295
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      3.52
_cell_volume                     2202.39(7)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEPIII (Burnett & Johnson, 1996)'
_computing_publication_material
'SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al.; 1999)'
_diffrn_ambient_temperature      295
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '\f scans and \w 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  0.0425
_diffrn_reflns_av_sigmaI/netI    0.0442
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            18140
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         3.52
_exptl_absorpt_coefficient_mu    1.077
_exptl_absorpt_correction_T_max  0.805
_exptl_absorpt_correction_T_min  0.645
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'SORTAV (R.H. Blessing, Acta Crystallogr., 1995, A51, 33)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.944
_refine_diff_density_min         -0.634
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         5301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+0.1402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1036
_refine_ls_wR_factor_ref         0.1115
_reflns_number_gt                4044
_reflns_number_total             5301
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            om900146a_si_002.cif
_cod_data_source_block           (3Et)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4069341