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_1556328
_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         'C23 H45 Cl2 N3 Pd1'
_chemical_formula_sum            'C23 H45 Cl2 N3 Pd'
_chemical_formula_weight         540.92
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_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
_cell_angle_alpha                90
_cell_angle_beta                 102.061(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7877(10)
_cell_length_b                   21.0937(13)
_cell_length_c                   8.1090(5)
_cell_measurement_reflns_used    9582
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      34.92
_cell_measurement_theta_min      2.34
_cell_measurement_wavelength     0.71073
_cell_volume                     2640.9(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    'Bruker SHELXTL'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.035
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            124677
_diffrn_reflns_theta_full        36.96
_diffrn_reflns_theta_max         36.96
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.919
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.912
_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    1.36
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     266
_refine_ls_number_reflns         13366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0311
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0224P)^2^+1.4003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0682
_reflns_number_gt                10115
_reflns_number_total             13366
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2cy20517c.txt
_cod_data_source_block           miguel140411
_cod_database_code               1556328