Nucleophilic addition of 1,3-dicarbonyl compounds as a route to functionalized cyclopalladated complexes with chelated 1,1-bis(diphenylphosphino)ethene
Roberto Mosteiro; Alberto Fernández; Margarita López-Torres; Digna Vázquez-García; Antonio Suárez; Jesús J. Fernández; José M. Vila; New J. Chem. 26 (2002) 1425–1432; doi:10.1039/b203864a

data_7050908
_publ_section_title
;
 Nucleophilic addition of 1,3-dicarbonyl compounds as a route to
 functionalized cyclopalladated complexes with chelated
 1,1-bis(diphenylphosphino)ethene
;
_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              1425
_journal_page_last               1432
_journal_paper_doi               10.1039/b203864a
_journal_volume                  26
_journal_year                    2002
_chemical_formula_sum            'C48 H54 F6 N O5 P3 Pd'
_chemical_formula_weight         1038.23
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.6610(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.0537(2)
_cell_length_b                   9.7220(3)
_cell_length_c                   23.33850(10)
_cell_measurement_temperature    293(2)
_cell_volume                     4776.70(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0670
_diffrn_reflns_av_sigmaI/netI    0.0844
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24120
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         0.97
_exptl_absorpt_coefficient_mu    0.558
_exptl_absorpt_correction_T_max  0.8965
_exptl_absorpt_correction_T_min  0.8075
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.857
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.868
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         8399
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      0.873
_refine_ls_R_factor_all          0.1069
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1149P)^2^+8.1276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1854
_reflns_number_gt                5249
_reflns_number_total             8399
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b203864a.txt
_cod_data_source_block           7
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 
;
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7050908