Room temperature asymmetric Pd-catalyzed methoxycarbonylation of norbornene: highly selective catalysis and HP-NMR studies.
Blanco, Carolina; Godard, Cyril; Zangrando, Ennio; Ruiz, Aurora; Claver, Carmen; Dalton transactions (Cambridge, England : 2003) 41 (2012) 6980–6991; doi:10.1039/c2dt30267e

data_7019375
_publ_section_title
;
 Room temperature asymmetric Pd-catalyzed methoxycarbonylation of
 norbornene: highly selective catalysis and HP-NMR studies.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6980
_journal_page_last               6991
_journal_paper_doi               10.1039/c2dt30267e
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C28 H48 Cl2 Fe P2 Pd C4 H8 O'
_chemical_formula_sum            'C32 H56 Cl2 Fe O P2 Pd'
_chemical_formula_weight         751.86
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.29(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.558(3)
_cell_length_b                   14.646(3)
_cell_length_c                   20.721(4)
_cell_measurement_reflns_used    394
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.55
_cell_measurement_theta_min      6.78
_cell_volume                     3497.8(13)
_computing_cell_refinement       'Denzo (Otwinowski & Minor 1997)'
_computing_data_collection       'XPRESS (MacScience, 2002)'
_computing_data_reduction
'Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep3 for Windows (Farrugia,1997)'
_computing_publication_material  'Wingx 1.80.05 (Farrugia, 1999)'
_computing_structure_refinement  'SHELX97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELX97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type
'Enraf-Nonius dip1030 image plate diffractometer'
_diffrn_measurement_method       '\f-scans 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  0.1362
_diffrn_reflns_av_sigmaI/netI    0.1183
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            42519
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    1.196
_exptl_absorpt_correction_T_max  1.0385
_exptl_absorpt_correction_T_min  0.4219
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Cubic fit to sin(theta)/lambda - 24 parameters
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.668
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.894
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         6015
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.1008
_refine_ls_R_factor_gt           0.0510
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1159
_refine_ls_wR_factor_ref         0.1354
_reflns_number_gt                3489
_reflns_number_total             6015
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c2dt30267e.txt
_cod_data_source_block           4a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7019375