Palladium catalytic systems with hybrid pyrazole ligands in C‒C coupling reactions. Nanoparticles versus molecular complexes
Peral, Daniel; Gómez-Villarraga, Fernando; Sala, Xavier; Pons, Josefina; Carles Bayón, J.; Ros, Josep; Guerrero, Miguel; Vendier, Laure; Lecante, Pierre; García-Antón, Jordi; Philippot, Karine; Catal. Sci. Technol. 3 (2013) 475–; doi:10.1039/C2CY20517C

data_1556325
_publ_section_title
;
 Palladium catalytic systems with hybrid pyrazole ligands in C--C coupling
 reactions. Nanoparticles versus molecular complexes
;
_journal_issue                   2
_journal_name_full               'Catal. Sci. Technol.'
_journal_page_first              475
_journal_paper_doi               10.1039/C2CY20517C
_journal_volume                  3
_journal_year                    2013
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C15 H29 Cl2 N3 Pd'
_chemical_formula_sum            'C15 H29 Cl2 N3 Pd'
_chemical_formula_weight         428.71
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_cell_angle_alpha                77.784(5)
_cell_angle_beta                 89.987(4)
_cell_angle_gamma                71.894(3)
_cell_formula_units_Z            4
_cell_length_a                   8.1051(8)
_cell_length_b                   11.1155(9)
_cell_length_c                   22.6264(6)
_cell_measurement_reflns_used    9500
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      32.5
_cell_measurement_theta_min      3.2
_cell_measurement_wavelength     0.71073
_cell_volume                     1888.9(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1993)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa APEX II'
_diffrn_measurement_method       \w-\f
_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  0.0177
_diffrn_reflns_av_unetI/netI     0.0118
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            41896
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.263
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.461
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         7685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0182
_refine_ls_R_factor_gt           0.0161
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0153P)^2^+1.1371P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0393
_refine_ls_wR_factor_ref         0.0409
_reflns_number_gt                7222
_reflns_number_total             7685
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2cy20517c.txt
_cod_data_source_block           miguel010411
_cod_original_cell_volume        1888.9(2)
_cod_database_code               1556325