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_4070116
_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            'C46 H46 F3 I N3 O4 P Pd S'
_chemical_formula_weight         1058.19
_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                82.160(2)
_cell_angle_beta                 84.779(3)
_cell_angle_gamma                86.690(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8654(5)
_cell_length_b                   13.2407(6)
_cell_length_c                   16.9801(8)
_cell_measurement_reflns_used    5545
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.31
_cell_volume                     2185.86(18)
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0342
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            25581
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    1.275
_exptl_absorpt_correction_T_max  0.9508
_exptl_absorpt_correction_T_min  0.8409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.608
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       lath
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.729
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment
'NH and water hydrogen free, rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         9836
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0306P)^2^+1.7446P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0698
_reflns_number_gt                8867
_reflns_number_total             9836
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900616v_si_002.cif
_cod_data_source_block           ajc44s
_cod_database_code               4070116