Synthesis and structural chemistry of N-{2-(arylthio/seleno) ethyl}morpholine/piperidine-palladium(II) complexes as potent catalysts for the Heck reaction
Pradhumn Singh; Dipanwita Das; Om Prakash; Ajai K. Singh; Inorganica Chimica Acta 393 (2012) 77–84; doi:

data_1512707
_publ_section_title
;
 Synthesis and structural chemistry of N-{2-(arylthio/seleno)
 ethyl}morpholine/piperidine-palladium(II) complexes as potent catalysts
 for the Heck reaction
;
_journal_name_full
;
Inorganica Chimica Acta
;
_journal_page_first              77
_journal_page_last               84
_journal_volume                  393
_journal_year                    2012
_chemical_formula_moiety         'C12 H17 Cl2 N O Pd S'
_chemical_formula_sum            'C12 H17 Cl2 N O Pd S'
_chemical_formula_weight         400.64
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   7.7390(19)
_cell_length_b                   9.812(2)
_cell_length_c                   37.950(9)
_cell_measurement_reflns_used    6256
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.84
_cell_volume                     2881.7(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  '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  0.0341
_diffrn_reflns_av_sigmaI/netI    0.0258
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            13411
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    1.790
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_correction_T_min  0.635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.847
_exptl_crystal_density_meas      1.852
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rods
_exptl_crystal_F_000             1600.0
_exptl_crystal_size_max          0.462
_exptl_crystal_size_mid          0.214
_exptl_crystal_size_min          0.164
_refine_diff_density_max         1.428
_refine_diff_density_min         -0.583
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         2517
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0411P)^2^+4.1076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0871
_reflns_number_gt                2320
_reflns_number_total             2517
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ICA-2013-394-77-84-4.cif
_cod_data_source_block           complex-1
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               1512707