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_4077898
_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            'C19 H19 F3 N2 O3 S'
_chemical_formula_weight         412.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 101.108(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.0508(9)
_cell_length_b                   8.7019(5)
_cell_length_c                   26.1081(14)
_cell_measurement_reflns_used    5201
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.11
_cell_measurement_theta_min      2.43
_cell_volume                     3801.2(4)
_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 0.999
_diffrn_measured_fraction_theta_max 0.941
_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  0.0200
_diffrn_reflns_av_sigmaI/netI    0.0165
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            21249
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    0.222
_exptl_absorpt_correction_T_max  0.9782
_exptl_absorpt_correction_T_min  0.8970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.441
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.460
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    'NH free, rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         4421
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0543P)^2^+6.6850P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1121
_refine_ls_wR_factor_ref         0.1145
_reflns_number_gt                4088
_reflns_number_total             4421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200986k_si_001.cif
_cod_data_source_block           ajd323s
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4077898