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_7050907
_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            'C41 H42 F6 N O2 P3 Pd'
_chemical_formula_weight         894.07
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                61.7800(10)
_cell_angle_beta                 64.0650(10)
_cell_angle_gamma                66.1710(10)
_cell_formula_units_Z            4
_cell_length_a                   16.9482(3)
_cell_length_b                   17.54900(10)
_cell_length_c                   18.0086(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4110.71(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0710
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22085
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.9113
_exptl_absorpt_correction_T_min  0.8583
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1824
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.121
_refine_diff_density_min         -0.727
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     973
_refine_ls_number_reflns         14094
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.1151
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0864P)^2^+9.2605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.2027
_reflns_number_gt                9254
_reflns_number_total             14094
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b203864a.txt
_cod_data_source_block           2
_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 

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'TRICLINIC' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4110.71(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050907