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_4083619
_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_compound_source        'synthesis as described'
_chemical_formula_moiety         'C54 H51 N4 O P3 Pd2 S, 2(Cl O4)'
_chemical_formula_sum            'C54 H51 Cl2 N4 O9 P3 Pd2 S'
_chemical_formula_weight         1308.66
_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             2009-04-22T18:49:39-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                79.370(5)
_cell_angle_beta                 68.872(5)
_cell_angle_gamma                81.035(5)
_cell_formula_units_Z            2
_cell_length_a                   12.6747(12)
_cell_length_b                   12.9371(13)
_cell_length_c                   17.4291(17)
_cell_measurement_reflns_used    1996
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.914
_cell_measurement_theta_min      2.4685
_cell_measurement_wavelength     0.71073
_cell_volume                     2607.6(5)
_computing_cell_refinement       "'BRUKER APEX2"
_computing_data_collection       "'BRUKER APEX2"
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.961
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0624
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            9720
_diffrn_reflns_theta_full        26.18
_diffrn_reflns_theta_max         26.18
_diffrn_reflns_theta_min         1.26
_exptl_absorpt_coefficient_mu    0.986
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.818
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1324
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.06
_refine_diff_density_max         2.1
_refine_diff_density_min         -1.308
_refine_diff_density_rms         0.19
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.229
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         9720
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.229
_refine_ls_R_factor_all          0.1236
_refine_ls_R_factor_gt           0.068
_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^)+(0.0314P)^2^+39.1195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1511
_refine_ls_wR_factor_ref         0.1856
_reflns_number_gt                6727
_reflns_number_total             9720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401069a_si_003.cif
_cod_data_source_block           vi09ji2n
_cod_original_cell_volume        2607.6(4)
_cod_database_code               4083619