New cyclopalladated benzothiophenes: a catalyst precursor for the Suzuki coupling of deactivated aryl chlorides.
Subhas, Madavu Salian; Racharlawar, Shailesh S.; Sridhar, B.; Kennady, P. Kavin; Likhar, Pravin R.; Kantam, Mannepalli Lakshmi; Bhargava, Suresh K.; Organic & biomolecular chemistry 8 (2010) 3001–3006; doi:10.1039/b927367k

data_7153325
_publ_section_title
;
 New cyclopalladated benzothiophenes: a catalyst precursor for the Suzuki
 coupling of deactivated aryl chlorides.
;
_journal_issue                   13
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              3001
_journal_page_last               3006
_journal_paper_doi               10.1039/b927367k
_journal_volume                  8
_journal_year                    2010
_chemical_formula_moiety         'C53 H41 Cl F3 N O P2 Pd S, C H Cl3, C Cl4'
_chemical_formula_sum            'C55 H42 Cl8 F3 N O P2 Pd S'
_chemical_formula_weight         1273.90
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                72.277(2)
_cell_angle_beta                 75.153(2)
_cell_angle_gamma                67.700(2)
_cell_formula_units_Z            2
_cell_length_a                   11.9921(15)
_cell_length_b                   13.0949(16)
_cell_length_c                   20.722(3)
_cell_measurement_reflns_used    8306
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      28.03
_cell_measurement_theta_min      2.39
_cell_volume                     2831.0(6)
_computing_cell_refinement       'SAINT (Bruker, 2001)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1990)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0273
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26905
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.04
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.848
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1284
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.906
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     648
_refine_ls_number_reflns         9947
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0558
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1037P)^2^+4.4516P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1595
_refine_ls_wR_factor_ref         0.1701
_reflns_number_gt                8673
_reflns_number_total             9947
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b927367k.txt
_cod_data_source_block           ae
_cod_database_code               7153325