Palladium(ii) complexes of pyrazolated thio/selenoethers: syntheses, structures, single source precursors of Pd(4)Se and PdSe nano-particles and potential for catalyzing Suzuki-Miyaura coupling.
Sharma, Kamal Nayan; Joshi, Hemant; Singh, Ved Vati; Singh, Pradhumn; Singh, Ajai Kumar; Dalton transactions (Cambridge, England : 2003) 42 (2013) 3908–3918; doi:10.1039/c2dt31975f

data_7020992
_publ_section_title
;
 Palladium(ii) complexes of pyrazolated thio/selenoethers: syntheses,
 structures, single source precursors of Pd(4)Se and PdSe nano-particles
 and potential for catalyzing Suzuki-Miyaura coupling.
;
_journal_issue                   11
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3908
_journal_page_last               3918
_journal_paper_doi               10.1039/c2dt31975f
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C10 H12 Br2 Cl N4 Pd Se, B F4'
_chemical_formula_sum            'C10 H12 B Br2 Cl F4 N4 Pd Se'
_chemical_formula_weight         655.66
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.924(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.142(4)
_cell_length_b                   11.090(3)
_cell_length_c                   11.001(3)
_cell_measurement_reflns_used    2825
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      24.65
_cell_measurement_theta_min      1.25
_cell_volume                     1800.5(8)
_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      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0398
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            16766
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    7.678
_exptl_absorpt_correction_T_max  0.264
_exptl_absorpt_correction_T_min  0.135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.419
_exptl_crystal_density_meas      2.419
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1232.0
_exptl_crystal_size_max          0.462
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.175
_refine_diff_density_max         1.544
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3169
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0367
_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^)+(0.0541P)^2^+4.9386P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.1006
_reflns_number_gt                2767
_reflns_number_total             3169
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31975f.txt
_cod_data_source_block           complex_4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7020992