Synthesis of 1,2-Dihydroquinazolinium-4-yl Palladium Complexes through a Cyclization Reaction
Vicente, José; Chicote, María Teresa; Martínez-Martínez, Antonio J.; Bautista, Delia; Organometallics 28 (2009) 5915–; doi:10.1021/om900616v

data_4070117
_publ_section_title
;
 Synthesis of 1,2-Dihydroquinazolinium-4-yl Palladium Complexes through a
 Cyclization Reaction
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              5915
_journal_paper_doi               10.1021/om900616v
_journal_volume                  28
_journal_year                    2009
_chemical_formula_sum            'C26 H27 Cl2 F3 I N3 O3 Pd S'
_chemical_formula_weight         822.77
_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                93.265(2)
_cell_angle_beta                 100.489(2)
_cell_angle_gamma                109.693(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2390(5)
_cell_length_b                   10.6933(5)
_cell_length_c                   15.2452(7)
_cell_measurement_reflns_used    7362
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.06
_cell_measurement_theta_min      2.30
_cell_volume                     1532.62(13)
_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 0.992
_diffrn_measured_fraction_theta_max 0.908
_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  0.0257
_diffrn_reflns_av_sigmaI/netI    0.0351
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17612
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    1.906
_exptl_absorpt_correction_T_max  0.9107
_exptl_absorpt_correction_T_min  0.7254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.125
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment
'NH2 free with SADI, NH free, mehtyls rigid others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     396
_refine_ls_number_reflns         6829
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0383P)^2^+1.0526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0768
_reflns_number_gt                6024
_reflns_number_total             6829
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900616v_si_002.cif
_cod_data_source_block           ajc431rs
_cod_database_code               4070117