Synthesis and Structure of PdII Complexes Containing the C,C-Chelating Bis-Ylide Ligand [Ph3PC(H)]2CO. X-ray Crystal Structure of {Pd(μ-Cl){[C(H)PPh3]2CO}}2(ClO4)2.CH2Cl2
Larry R. Falvello; Susana Fernández; Rafael Navarro; Angel Rueda; Esteban P. Urriolabeitia; Inorganic Chemistry 37 (1998) 6007–6013; doi:10.1021/ic980392z

data_4323161
_publ_section_title
;
 Synthesis and Structure of PdII Complexes Containing the C,C-Chelating
 Bis-Ylide Ligand [Ph3PC(H)]2CO. X-ray Crystal Structure of
 {Pd(\m-Cl){[C(H)PPh3]2CO}}2(ClO4)2.CH2Cl2
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6007
_journal_page_last               6013
_journal_paper_doi               10.1021/ic980392z
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C79 H66 Cl6 O10 P4 Pd2'
_chemical_formula_weight         1724.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.247(5)
_cell_length_b                   19.521(4)
_cell_length_c                   19.757(4)
_cell_measurement_temperature    150(2)
_cell_volume                     7423(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1028
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7107
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.860
_exptl_crystal_density_diffrn    1.543
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3496
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.054
_refine_diff_density_min         -1.214
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.09(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     904
_refine_ls_number_reflns         7107
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0579
_refine_ls_shift/su_max          0.083
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+17.4882P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1223
_refine_ls_wR_factor_ref         0.1413
_reflns_number_gt                5298
_reflns_number_total             7107
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980392z.cif
_cod_data_source_block           x
_cod_depositor_comments
;
The following automatic conversions were performed:

'_geom_angle_publ_flag' value 'Y' changed to 'y' 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 1673 2011-04-08 12:14:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0536P)^2^+17.4882P] 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^)+(0.0536P)^2^+17.4882P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323161