Synthesis of β-Imino Carbonyl Enolato Complexes by Reaction of Nickel(II), Palladium(II), and Copper(II) Acetates with the Enaminodiones (MeOCO)(RCO)CC(R')NH2 (R = Me, OMe; R' = Et, EtOCO)
Marino Basato; Umberto Vettori; Augusto C. Veronese; Alfonso Grassi; Giovanni Valle; Inorganic Chemistry 37 (1998) 6737–6745; doi:10.1021/ic9716114

data_4323236
_publ_section_title
;
 Synthesis of \b-Imino Carbonyl Enolato Complexes by Reaction of
 Nickel(II), Palladium(II), and Copper(II) Acetates with the Enaminodiones
 (MeOCO)(RCO)CC(R')NH2 (R = Me, OMe; R' = Et, EtOCO)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6737
_journal_page_last               6745
_journal_paper_doi               10.1021/ic9716114
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         'C16 H24 N2 O8 Pd'
_chemical_formula_sum            'C16 H24 N2 O8 Pd'
_chemical_formula_weight         478.77
_chemical_name_systematic
;
bis(3-imino-1-methoxy-2-methoxycarbonyl-1,4-pentanedionato-N2,O4)palladium
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXN ADAPTED TO SHELX76'
_cell_angle_alpha                90.00
_cell_angle_beta                 94.20(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.963(2)
_cell_length_b                   8.438(1)
_cell_length_c                   19.637(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      7
_cell_volume                     1976.9(5)
_computing_structure_refinement  'SHELXL76 (Sheldrick, 1976)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Philips PW 1100 diffractometer'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.01
_diffrn_reflns_av_sigmaI/netI    0.4305
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3586
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.05
_diffrn_standards_decay_%        10
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  variable
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.0983
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.61
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   0.688
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         2981
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.041
_refine_ls_shift/esd_max         0.363
_refine_ls_shift/esd_mean        0.0554
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/[\s^2^(F)+0.009245(F^2^)]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.047
_reflns_number_gt                2981
_reflns_number_total             3304
_reflns_observed_criterion       >3sigma(F)
_cod_data_source_file            ic9716114_1.cif
_cod_data_source_block           7b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(F)+0.009245(F^2^)]' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w=1/[\s^2^(F)+0.009245(F^2^)]'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4323236