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_4083620
_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 O2 P3 Pd2 S, 2(Cl O4), 4(C H Cl3)'
_chemical_formula_sum            'C58 H55 Cl14 N4 O10 P3 Pd2 S'
_chemical_formula_weight         1802.13
_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             2009-04-20T18:28:08-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                71.881(5)
_cell_angle_beta                 84.511(5)
_cell_angle_gamma                79.138(5)
_cell_formula_units_Z            2
_cell_length_a                   11.207(5)
_cell_length_b                   17.086(5)
_cell_length_c                   19.644(5)
_cell_measurement_reflns_used    1602
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      22.408
_cell_measurement_theta_min      2.45
_cell_volume                     3508(2)
_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      100.0(1)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0879
_diffrn_reflns_av_unetI/netI     0.1149
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13232
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         1.09
_exptl_absorpt_coefficient_mu    1.202
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.853
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER SADABS'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1804
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.077
_refine_diff_density_min         -1.287
_refine_diff_density_rms         0.182
_refine_ls_extinction_coef       0.0012(2)
_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   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     834
_refine_ls_number_reflns         13232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.1321
_refine_ls_R_factor_gt           0.0661
_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^)+(0.0704P)^2^+24.7113P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1807
_reflns_number_gt                8043
_reflns_number_total             13232
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om401069a_si_003.cif
_cod_data_source_block           vi06ji2n
_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               4083620