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_4083617
_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         'C29 H29 N4 O2 P Pd S'
_chemical_formula_sum            'C29 H29 N4 O2 P Pd S'
_chemical_formula_weight         634.99
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_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
_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             2009-04-16T18:18:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                80.959(5)
_cell_angle_beta                 84.527(5)
_cell_angle_gamma                74.360(5)
_cell_formula_units_Z            2
_cell_length_a                   8.894(5)
_cell_length_b                   9.756(5)
_cell_length_c                   16.809(5)
_cell_measurement_reflns_used    1428
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.04
_cell_measurement_theta_min      2.51
_cell_volume                     1384.9(11)
_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, 1997)'
_computing_structure_solution    'SIR97 (Altomare et all, 1999)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.98
_diffrn_measurement_device_type  'Smart-CCD-1000 BRUKER'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0787
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            10806
_diffrn_reflns_theta_full        28.3
_diffrn_reflns_theta_max         28.3
_diffrn_reflns_theta_min         1.23
_exptl_absorpt_coefficient_mu    0.837
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.523
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.848
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     351
_refine_ls_number_reflns         4340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.748
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0759
_reflns_number_gt                3313
_reflns_number_total             6645
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401069a_si_003.cif
_cod_data_source_block           vi01ji1n
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_database_code               4083617