Synthesis and reactivity of palladium hydrido-solvento complexes, including a key intermediate in the catalytic methoxycarbonylation of ethene to methyl propanoate
Clegg, William; Eastham, Graham R.; Elsegood, Mark R. J.; Heaton, Brian T.; Iggo, Jonathan A.; Tooze, Robert P.; Whyman, Robin; Zacchini, Stefano; Journal of the Chemical Society, Dalton Transactions  (2002) 3300–; doi:10.1039/b202372p

data_7011636
_publ_section_title
;
 Synthesis and reactivity of palladium hydrido-solvento complexes,
 including a key intermediate in the catalytic methoxycarbonylation of
 ethene to methyl propanoate
;
_journal_issue                   17
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3300
_journal_paper_doi               10.1039/b202372p
_journal_year                    2002
_chemical_formula_sum            'C59 H90 O9 P2 Pd S2'
_chemical_formula_weight         1175.95
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           2
_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                72.45(3)
_cell_angle_beta                 85.34(3)
_cell_angle_gamma                65.79(2)
_cell_formula_units_Z            2
_cell_length_a                   14.422(3)
_cell_length_b                   15.236(3)
_cell_length_c                   15.695(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2995.4(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_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  0.0863
_diffrn_reflns_av_sigmaI/netI    0.0885
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15324
_diffrn_reflns_theta_full        22.39
_diffrn_reflns_theta_max         22.39
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    0.423
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1248
_refine_diff_density_max         0.962
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.970
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     672
_refine_ls_number_reflns         7168
_refine_ls_number_restraints     86
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0984P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1353
_refine_ls_wR_factor_ref         0.1403
_reflns_number_gt                5845
_reflns_number_total             7168
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b202372p.txt
_cod_data_source_block           zac2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0984P)^2^+0.0000P] 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^)+(0.0984P)^2^+0.0000P] 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        2995.6(11)
_cod_database_code               7011636