Highly active and selective catalysts for the production of methyl propanoate via the methoxycarbonylation of ethene
Clegg, William; Elsegood, Mark R. J.; Eastham, Graham R.; Tooze, Robert P.; Wang, Xiao Lan; Whiston, Keith; Chemical Communications  (1999) 1877–; doi:10.1039/a905521e

data_7110648
_publ_section_title
;
 Highly active and selective catalysts for the production of methyl
 propanoate via the methoxycarbonylation of ethene
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              1877
_journal_paper_doi               10.1039/a905521e
_journal_year                    1999
_chemical_formula_sum            'C102.5 H213 Cl21 O16 P8 Pd4'
_chemical_formula_weight         3119.54
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 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                   38.530(2)
_cell_length_b                   19.1969(9)
_cell_length_c                   20.3787(10)
_cell_measurement_reflns_used    40041
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.85
_cell_measurement_theta_min      2.11
_cell_volume                     15073.2(13)
_computing_cell_refinement       'local programs'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'Siemens SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.1008
_diffrn_reflns_av_sigmaI/netI    0.1372
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            91913
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.90
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.976
_exptl_absorpt_correction_T_max  0.802
_exptl_absorpt_correction_T_min  0.388
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             6468
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.411
_refine_diff_density_min         -1.387
_refine_diff_density_rms         0.144
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(2)
_refine_ls_extinction_coef       0.00019(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1420
_refine_ls_number_reflns         33354
_refine_ls_number_restraints     287
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.1329
_refine_ls_R_factor_gt           0.0723
_refine_ls_shift/su_max          0.060
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+16.4146P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1680
_reflns_number_gt                21570
_reflns_number_total             33354
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            905521esup1.cif
_cod_data_source_block           exti51
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               7110648