Mononuclear palladium and heterodinuclear palladium–ruthenium complexes of semicarbazone ligands. Synthesis, characterization, and application in C–C cross-coupling reactions
Datta, Sayanti; Kumar Seth, Dipravath; Halder, Sarmistha; Sheldrick, William S.; Mayer-Figge, Heike; Drew, Michael G. B.; Bhattacharya, Samaresh; RSC Advances 2 (2012) 5254–; doi:10.1039/c2ra20105d

data_7238610
_publ_section_title
;
 Mononuclear palladium and heterodinuclear palladium--ruthenium complexes
 of semicarbazone ligands. Synthesis, characterization, and application in
 C--C cross-coupling reactions
;
_journal_issue                   12
_journal_name_full               'RSC Advances'
_journal_page_first              5254
_journal_paper_doi               10.1039/c2ra20105d
_journal_volume                  2
_journal_year                    2012
_chemical_formula_sum            'C27 H24 N3 O2 P Pd'
_chemical_formula_weight         554.86
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                80.414(7)
_cell_angle_beta                 84.706(7)
_cell_angle_gamma                78.503(7)
_cell_formula_units_Z            4
_cell_length_a                   10.1264(9)
_cell_length_b                   14.1165(12)
_cell_length_c                   16.8322(12)
_cell_measurement_temperature    150(2)
_cell_volume                     2320.6(3)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_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  0.0293
_diffrn_reflns_av_sigmaI/netI    0.1335
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            16582
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.900
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.801
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.116
_refine_diff_density_min         -0.810
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.931
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     615
_refine_ls_number_reflns         13031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.931
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
_refine_ls_weighting_details
w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                7296
_reflns_number_total             13031
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ra20105d.txt
_cod_data_source_block           x
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7238610