Insertion Reactions into Pd-O and Pd-N Bonds: Preparation of Alkoxycarbonyl, Carbonato, Carbamato, Thiocarbamate, and Thioureide Complexes of Palladium(II)
José Ruiz; M. Teresa Martínez; Félix Florenciano; Venancio Rodríguez; Gregorio López; José Pérez; Penny A. Chaloner; Peter B. Hitchcock; Inorganic Chemistry 42 (2003) 3650–3661; doi:10.1021/ic0300058

data_4313707
_publ_section_title
;
 Insertion Reactions into Pd-O and Pd-N Bonds: Preparation of
 Alkoxycarbonyl, Carbonato, Carbamato, Thiocarbamate, and Thioureide
 Complexes of Palladium(II)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3650
_journal_page_last               3661
_journal_paper_doi               10.1021/ic0300058
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C39 H28 Cl4 F10 N4 O3 Pd2'
_chemical_formula_weight         1145.25
_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                70.810(4)
_cell_angle_beta                 84.557(4)
_cell_angle_gamma                84.114(4)
_cell_formula_units_Z            2
_cell_length_a                   11.1311(6)
_cell_length_b                   11.6741(7)
_cell_length_c                   17.0116(8)
_cell_measurement_reflns_used    54
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.45
_cell_measurement_theta_min      7.43
_cell_volume                     2072.3(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_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  0.0157
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10850
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.215
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.869
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     564
_refine_ls_number_reflns         7209
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.871
_refine_ls_R_factor_all          0.0427
_refine_ls_R_factor_gt           0.0323
_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^)+(0.0660P)^2^+1.4193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0829
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                5917
_reflns_number_total             7209
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0300058_2.cif
_cod_data_source_block           complex13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        2072.34(19)
_cod_database_code               4313707