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_4065184
_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            'C94.5 H81 Cl3 I2 P4 Pd2 S2'
_chemical_formula_weight         1977.54
_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                69.526(5)
_cell_angle_beta                 88.976(5)
_cell_angle_gamma                82.322(5)
_cell_formula_units_Z            2
_cell_length_a                   14.505(2)
_cell_length_b                   17.404(3)
_cell_length_c                   18.296(3)
_cell_measurement_reflns_used    9336
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      30.42
_cell_measurement_theta_min      2.34
_cell_volume                     4286.1(12)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.0797
_diffrn_reflns_av_sigmaI/netI    0.0986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            78661
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.19
_exptl_absorpt_coefficient_mu    1.402
_exptl_absorpt_correction_T_max  0.8961
_exptl_absorpt_correction_T_min  0.7400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1978
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.769
_refine_diff_density_min         -1.497
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    'rigid methyls, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     997
_refine_ls_number_reflns         21156
_refine_ls_number_restraints     365
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1152
_refine_ls_R_factor_gt           0.0643
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0586P)^2^+13.9854P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1503
_reflns_number_gt                13352
_reflns_number_total             21156
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200607h_si_001.cif
_cod_data_source_block           thring
_cod_depositor_comments
'Adding full bibliography for 4065180--4065189.cif.'
_cod_original_cell_volume        4286.2(12)
_cod_original_formula_sum        'C94.50 H81 Cl3 I2 P4 Pd2 S2'
_cod_database_code               4065184