Synthesis and Characterization of {Pd(dmba)(py)[OC(CH3)C(H)PPh3]}(ClO4).CH2Cl2. Unusual O-Coordination of the (Acetylmethylene)triphenylphosphorane Ligand to a Soft Metal Center
Larry R. Falvello; Susana Fernández; Rafael Navarro; Esteban P. Urriolabeitia; Inorganic Chemistry 35 (1996) 3064–3066; doi:10.1021/ic951311r

data_4323814
_publ_section_title
;
 Synthesis and Characterization of
 {Pd(dmba)(py)[OC(CH3)C(H)PPh3]}(ClO4).CH2Cl2. Unusual O-Coordination of
 the (Acetylmethylene)triphenylphosphorane Ligand to a Soft Metal Center
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3064
_journal_page_last               3066
_journal_paper_doi               10.1021/ic951311r
_journal_volume                  35
_journal_year                    1996
_chemical_formula_sum            'C36 H38 Cl3 N2 O5 P Pd'
_chemical_formula_weight         822.40
_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
_cell_angle_alpha                75.103(5)
_cell_angle_beta                 81.255(4)
_cell_angle_gamma                85.308(3)
_cell_formula_units_Z            2
_cell_length_a                   11.1353(5)
_cell_length_b                   12.7720(8)
_cell_length_c                   13.5235(8)
_cell_measurement_temperature    298(2)
_cell_volume                     1835.22(18)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_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  0.0156
_diffrn_reflns_av_sigmaI/netI    0.0374
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            6818
_diffrn_reflns_theta_max         24.96
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.811
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_F_000             840
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.068
_refine_ls_goodness_of_fit_obs   1.104
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         6426
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.071
_refine_ls_restrained_S_obs      1.106
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_obs          0.0370
_refine_ls_shift/esd_max         -0.026
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+0.6672P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0927
_refine_ls_wR_factor_obs         0.0890
_reflns_number_observed          5606
_reflns_number_total             6426
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic951311r.cif
_cod_data_source_block           IC951311R
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+0.6672P] 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^)+(0.0419P)^2^+0.6672P] 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        1835.2(2)
_cod_database_code               4323814