Bis(N-substituted oxamate)palladate(ii) complexes as effective catalysts for sustainable Heck carbon‒carbon coupling reactions in n-Bu4NBr as the solvent
Fortea-Pérez, Francisco Ramón; Rothenpieler, Berit L.; Marino, Nadia; Armentano, Donatella; De Munno, Giovanni; Julve, Miguel; Stiriba, Salah-Eddine; Inorganic Chemistry Frontiers 2 (2015) 1029–; doi:10.1039/C5QI00093A

data_4348946
_publ_section_title
;
 Bis(N-substituted oxamate)palladate(ii) complexes as effective catalysts
 for sustainable Heck carbon--carbon coupling reactions in n-Bu4NBr as the
 solvent
;
_journal_issue                   11
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1029
_journal_paper_doi               10.1039/C5QI00093A
_journal_volume                  2
_journal_year                    2015
_chemical_formula_moiety
'3(C16 H8 Br2 N2 O6 Pd), 6(C16 H36 N), 3(H2 O)'
_chemical_formula_sum            'C144 H234 Br6 N12 O21 Pd3'
_chemical_formula_weight         3268.08
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-05-22 deposited with the CCDC.
2015-09-14 downloaded from the CCDC.
;
_cell_angle_alpha                100.901(8)
_cell_angle_beta                 103.304(8)
_cell_angle_gamma                99.809(8)
_cell_formula_units_Z            1
_cell_length_a                   13.524(2)
_cell_length_b                   16.287(3)
_cell_length_c                   20.967(3)
_cell_measurement_reflns_used    9575
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.35
_cell_measurement_theta_min      2.17
_cell_volume                     4301.3(12)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0508
_diffrn_reflns_av_unetI/netI     0.0589
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            88674
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.732
_diffrn_reflns_theta_min         1.457
_exptl_absorpt_coefficient_mu    1.762
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6722
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 - Bruker AXS'
_exptl_crystal_colour            pale-yellow
_exptl_crystal_density_diffrn    1.262
_exptl_crystal_description       prism
_exptl_crystal_F_000             1698
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     992
_refine_ls_number_reflns         18125
_refine_ls_number_restraints     956
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1243
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1255P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1750
_refine_ls_wR_factor_ref         0.2121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9794
_reflns_number_total             18125
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5qi00093a2.cif
_cod_data_source_block           3
_cod_original_cell_volume        4301.1(13)
_cod_database_code               4348946
_shelx_estimated_absorpt_t_min   0.719
_shelx_estimated_absorpt_t_max   0.843
_shelxl_version_number           2013-4
_shelx_res_checksum              78772
_shelx_hkl_checksum              98977