Reactivity of Palladium(II) Complexes Containing the Orthometalated C,C-Chelating Ligand C6H4-2-PPh2C(H)COCH2PPh3 toward Deprotonating Reagents
Larry R. Falvello; Susana Fernández; Rafael Navarro; Esteban P. Urriolabeitia; Inorganic Chemistry 38 (1999) 2455–2463; doi:10.1021/ic9812050

data_4322013
_publ_section_title
;
 Reactivity of Palladium(II) Complexes Containing the Orthometalated
 C,C-Chelating Ligand C6H4-2-PPh2C(H)COCH2PPh3 toward Deprotonating
 Reagents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2455
_journal_page_last               2463
_journal_paper_doi               10.1021/ic9812050
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C78 H62 Cl4 Hg O10 P4 Pd2'
_chemical_formula_weight         1838.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 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                 90.333(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.205(3)
_cell_length_b                   11.7529(9)
_cell_length_c                   30.905(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      14.39
_cell_measurement_theta_min      11.12
_cell_volume                     7338.8(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.473
_diffrn_measured_fraction_theta_max 0.473
_diffrn_measurement_device_type  'NONIUS CAD-4'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_sigmaI/netI    0.1350
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            6584
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         2.00
_diffrn_standards_interval_time  30
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.863
_exptl_absorpt_correction_T_max  0.95117
_exptl_absorpt_correction_T_min  0.83056
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            prism
_exptl_crystal_density_diffrn    1.664
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       yellow
_exptl_crystal_F_000             3640
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.030
_refine_diff_density_min         -0.636
_refine_diff_density_rms         0.163
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         6418
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1410
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+37.0009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1355
_reflns_number_gt                4103
_reflns_number_total             6418
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9812050.cif
_cod_data_source_block           cad4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0338P)^2^+37.0009P] where P=(Fo^2^+2Fc^2^)/3'
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^(Fo^2^)+(0.0338P)^2^+37.0009P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        7339.0(14)
_cod_database_code               4322013