Novel Bidentate [N,S] Palladacycle Metalloligands.1H‒15N HMBC as a Decisive NMR Technique for the Structural Characterization of Palladium‒Rhodium and Palladium‒Palladium Bimetallic Complexes
Pereira, M. Teresa; Antelo, José M.; Adrio, Luis A.; Martínez, Javier; Ortigueira, Juan M.; López-Torres, Margarita; Vila, José M.; Organometallics  (2014) 140612083847005–; doi:10.1021/om401069a

data_4083618
_publ_section_title
;
 Novel Bidentate [N,S] Palladacycle Metalloligands.1H--15N HMBC as a
 Decisive NMR Technique for the Structural Characterization of
 Palladium--Rhodium and Palladium--Palladium Bimetallic Complexes
;
_journal_name_full               Organometallics
_journal_page_first              140612083847005
_journal_paper_doi               10.1021/om401069a
_journal_year                    2014
_chemical_formula_moiety         'C28 H27 N4 P Pd S, C3 H6 O '
_chemical_formula_sum            'C31 H33 N4 O P Pd S'
_chemical_formula_weight         647.04
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2006-03-20T17:50:13-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                103.130(5)
_cell_angle_beta                 99.996(5)
_cell_angle_gamma                92.067(5)
_cell_formula_units_Z            2
_cell_length_a                   9.663(5)
_cell_length_b                   11.932(5)
_cell_length_c                   13.589(5)
_cell_measurement_reflns_used    9049
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.37
_cell_measurement_theta_min      2.41
_cell_volume                     1498.0(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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.607
_diffrn_measured_fraction_theta_max 0.607
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0641
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9892
_diffrn_reflns_theta_full        26.42
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         1.57
_exptl_absorpt_coefficient_mu    0.773
_exptl_absorpt_correction_T_max  0.837
_exptl_absorpt_correction_T_min  0.778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker-SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.24
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       0.0002(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.832
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         3725
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.832
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0194P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0558
_refine_ls_wR_factor_ref         0.0586
_reflns_number_gt                2989
_reflns_number_total             3725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401069a_si_003.cif
_cod_data_source_block           vi13ji1n
_cod_database_code               4083618