Synthesis and Reactivity of [PdCl2{C,N-C6H4C(═NHXy)NH2-2}] and Neutral Palladium 1,2-Dihydroquinazolinium-4-yl Complexes: Depalladation Reactions
Mart\?ínez-Martínez, Antonio-Jesús; Vicente, José; Chicote, Mar\?ía-Teresa; Bautista, Delia; Organometallics 31 (2012) 2697–; doi:10.1021/om200986k

data_4077896
_publ_section_title
;
 Synthesis and Reactivity of [PdCl2{C,N-C6H4C(&#x2550;NHXy)NH2-2}] and
 Neutral Palladium 1,2-Dihydroquinazolinium-4-yl Complexes: Depalladation
 Reactions
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              2697
_journal_paper_doi               10.1021/om200986k
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C36.5 H39.5 Cl3 N2 O4.75 P Pd'
_chemical_formula_weight         825.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.173(2)
_cell_angle_beta                 83.977(2)
_cell_angle_gamma                68.880(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3406(9)
_cell_length_b                   11.5447(9)
_cell_length_c                   14.9407(11)
_cell_measurement_reflns_used    7855
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.49
_cell_measurement_theta_min      2.25
_cell_volume                     1814.0(2)
_computing_cell_refinement       'BRUKER SAINT'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SAINT'
_computing_molecular_graphics    'BRUKER SHELXTL'
_computing_publication_material  'BRUKER SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.26
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.904
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       \w-scan
_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  0.0197
_diffrn_reflns_av_sigmaI/netI    0.0247
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22228
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.71
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  0.9008
_exptl_absorpt_correction_T_min  0.7129
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             845
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.137
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    'NH2 free with DFIX, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         8491
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0329P)^2^+4.5567P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1002
_reflns_number_gt                8355
_reflns_number_total             8491
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200986k_si_001.cif
_cod_data_source_block           aje62s
_cod_original_cell_volume        1814.1(2)
_cod_original_formula_sum        'C36.50 H39.50 Cl3 N2 O4.75 P Pd'
_cod_database_code               4077896