Palladated Oligophenylene Thioethers: Synthesis and Reactivity toward Isocyanides, Carbon Monoxide, and Alkynes
Vicente, José; Abad, José Antonio; López-Nicolás, Rosa-María; Jones, Peter G.; Organometallics 30 (2011) 4983–; doi:10.1021/om200607h

data_4065183
_publ_section_title
;
 Palladated Oligophenylene Thioethers: Synthesis and Reactivity toward
 Isocyanides, Carbon Monoxide, and Alkynes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4983
_journal_paper_doi               10.1021/om200607h
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C67 H64 Br2 Cl2 P2 Pd2 S2'
_chemical_formula_weight         1438.76
_chemical_name_systematic
;

 ?

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 105.56(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.203(3)
_cell_length_b                   15.410(3)
_cell_length_c                   22.325(4)
_cell_measurement_reflns_used    4862
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      29.3
_cell_measurement_theta_min      2.1
_cell_volume                     6033(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Siemens XP'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       '\w- & \f-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  0.0920
_diffrn_reflns_av_sigmaI/netI    0.0832
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            62445
_diffrn_reflns_theta_full        26.25
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.16
_exptl_absorpt_coefficient_mu    2.173
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.814
_refine_diff_density_min         -1.528
_refine_diff_density_rms         0.144
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     659
_refine_ls_number_reflns         12344
_refine_ls_number_restraints     197
_refine_ls_restrained_S_all      0.979
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0743P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1394
_reflns_number_gt                7860
_reflns_number_total             12344
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200607h_si_001.cif
_cod_data_source_block           shnay
_cod_depositor_comments
'Adding full bibliography for 4065180--4065189.cif.'
_cod_original_cell_volume        6032.6(19)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4065183