Catalytic Properties of [Pd(COOMe)nX2-n(PPh3)2] (n= 0, 1, 2; X = Cl, NO2, ONO2, OAc and OTs) in the Oxidative Carbonylation of MeOH
Emanuele Amadio; Gianni Cavinato; Alessandro Dolmella; Luigi Toniolo; Inorganic Chemistry 49 (2010) 3721–3729; doi:10.1021/ic901569w

data_4315355
_publ_section_title
;
 Catalytic Properties of [Pd(COOMe)nX2-n(PPh3)2] (n= 0, 1, 2; X = Cl, NO2,
 ONO2, OAc and OTs) in the Oxidative Carbonylation of MeOH
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3721
_journal_page_last               3729
_journal_paper_doi               10.1021/ic901569w
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C38 H33 N O5 P2 Pd'
_chemical_formula_weight         751.99
_chemical_name_systematic
;
 trans-(methoxycarbonyl)-(nitrato,O)-bis(triphenylphosphine)-palladium(II)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 91.85(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.011(3)
_cell_length_b                   19.446(3)
_cell_length_c                   16.276(3)
_cell_measurement_reflns_used    30
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      15.3
_cell_measurement_theta_min      12.1
_cell_volume                     3483.2(13)
_computing_cell_refinement       'FEBO system'
_computing_data_collection       'FEBO system'
_computing_data_reduction        'FEBO system'
_computing_molecular_graphics    'WinGX 1.70.00 (Farrugia, 1999)'
_computing_publication_material  'SHELXTL NT vers.5.10 (Sheldrick, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al. 1999)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Philips PW1100 dffractometer'
_diffrn_measurement_method       'omega-2 theta'
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7048
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  0.906
_exptl_absorpt_correction_T_min  0.876
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prisms
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.14(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         6803
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.093
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0135P)^2^+8.7399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1050
_reflns_number_gt                6306
_reflns_number_total             6803
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901569w_si_001_1.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
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_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4315355