Hybrid Thiophosphoryl‒Benzothiazole Palladium SCN-Pincer Complexes: Synthesis and Effect of Structure Modifications on Catalytic Performance in the Suzuki Cross-Coupling
Kozlov, Vladimir A.; Aleksanyan, Diana V.; Nelyubina, Yulia V.; Lyssenko, Konstantin A.; Petrovskii, Pavel V.; Vasil’ev, Andrei A.; Odinets, Irina L.; Organometallics 30 (2011) 2920–; doi:10.1021/om101012r

data_4063884
_publ_section_title
;
 Hybrid Thiophosphoryl--Benzothiazole Palladium SCN-Pincer Complexes:
 Synthesis and Effect of Structure Modifications on Catalytic Performance
 in the Suzuki Cross-Coupling
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2920
_journal_paper_doi               10.1021/om101012r
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         '2(C25 H17 Cl N P Pd S2), C H2 Cl2'
_chemical_formula_sum            'C51 H36 Cl4 N2 P2 Pd2 S4'
_chemical_formula_weight         1221.60
_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                71.5290(10)
_cell_angle_beta                 82.3750(11)
_cell_angle_gamma                69.1980(10)
_cell_formula_units_Z            1
_cell_length_a                   9.6828(6)
_cell_length_b                   11.1434(6)
_cell_length_c                   12.3807(7)
_cell_measurement_reflns_used    2668
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      3
_cell_volume                     1184.15(12)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'APEX2 (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_publication_material  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_refinement  'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_computing_structure_solution    'SHELXTL ver. 5.1 (Sheldrick, 1998b)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13105
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    1.269
_exptl_absorpt_correction_T_max  0.886
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'APEX2 (Bruker, 2005)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             610
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.481
_refine_diff_density_min         -0.986
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5685
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0277
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0660
_refine_ls_wR_factor_ref         0.0678
_reflns_number_gt                4982
_reflns_number_total             5685
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            om101012r_si_001.cif
_cod_data_source_block           12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               4063884