Mono-, Di-, and Trinuclear Palladium(II) Complexes Containing a Ligand with One, Two, or Three 1,2-Dihydroquinazolinium-4-yl Groups
Vicente, José; Chicote, María Teresa; Martínez-Martínez, Antonio J.; Bautista, Delia; Organometallics 30 (2011) 2425–; doi:10.1021/om200188r

data_4064587
_publ_section_title
;
 Mono-, Di-, and Trinuclear Palladium(II) Complexes Containing a Ligand
 with One, Two, or Three 1,2-Dihydroquinazolinium-4-yl Groups
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              2425
_journal_paper_doi               10.1021/om200188r
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C77 H72 Cl2 F6 I2 N8 O6 Pd2 S2'
_chemical_formula_weight         1921.05
_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                93.652(2)
_cell_angle_beta                 96.824(2)
_cell_angle_gamma                97.606(2)
_cell_formula_units_Z            2
_cell_length_a                   9.5852(6)
_cell_length_b                   16.1945(7)
_cell_length_c                   26.5651(12)
_cell_measurement_reflns_used    6492
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.00
_cell_measurement_theta_min      2.20
_cell_volume                     4045.2(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTLT'
_computing_publication_material  'Bruker SHELXTLT'
_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 0.905
_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  0.0546
_diffrn_reflns_av_sigmaI/netI    0.0788
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            46767
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    1.394
_exptl_absorpt_correction_T_max  0.9087
_exptl_absorpt_correction_T_min  0.7969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1912
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.524
_refine_diff_density_min         -1.196
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment
;
NH refined with DFIx,H06 with fixed temperature factors
rigid methyls others riding
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     965
_refine_ls_number_reflns         18134
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0714
_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^)+(0.0478P)^2^+13.2591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1458
_reflns_number_gt                13652
_reflns_number_total             18134
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200188r_si_002.cif
_cod_data_source_block           ajd111s
_cod_database_code               4064587