Concepts for Stereoselective Acrylate Insertion
Boris Neuwald; Lucia Caporaso; Luigi Cavallo; Stefan Mecking; Journal of the American Chemical Society 135 (2013) 1026–1036; doi:10.1021/ja3101787

data_4119208
_publ_contact_author_address
;Chair of Chemical Materials Science; 
Department of Chemistry 
University of Konstanz; 
78464 Konstanz 
Germany
;
_publ_contact_author_email       Stefan.Mecking@uni-konstanz.de
_publ_contact_author_fax         '+49 7531 88-5152'
_publ_contact_author_name        'Prof. Dr. Stefan Mecking'
_publ_contact_author_phone       '+49 7531 88-5151'
_publ_section_title
;
 Concepts for Stereoselective Acrylate Insertion
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1026
_journal_page_last               1036
_journal_paper_doi               10.1021/ja3101787
_journal_volume                  135
_journal_year                    2013
_chemical_formula_sum            'C34 H40 N O6 P Pd S'
_chemical_formula_weight         728.10
_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-97
_cell_angle_alpha                83.646(3)
_cell_angle_beta                 72.284(3)
_cell_angle_gamma                80.759(3)
_cell_formula_units_Z            4
_cell_length_a                   14.9093(6)
_cell_length_b                   15.1538(7)
_cell_length_c                   18.8836(8)
_cell_measurement_reflns_used    47384
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      1.88
_cell_volume                     4002.7(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED32'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.0752
_diffrn_reflns_av_sigmaI/netI    0.0722
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            58103
_diffrn_reflns_theta_full        26.84
_diffrn_reflns_theta_max         26.84
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_T_max  0.9201
_exptl_absorpt_correction_T_min  0.8481
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED32'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       plate
_exptl_crystal_F_000             1504
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.050
_platon_squeeze_details
;
 
 Toluene was detected in at least three independent positions in the asymmetric 
 unit close to the centre of symmetry and could not be satisfactorily modeled 
 due to disorder.
 Further improvement was achieved using the SQUEEZE routine implemented
 in PLATON (Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13) by which
 323 e- (four molecules toluene) were removed in a 998 cubic Ang solvent 
 accessible void from the reflection data.
 Results of the SQUEEZE routine are preceding.
 The calculated density and F000 are based on the toluene free structure.
 However, absorption correction was applied assuming four molecules
 of toluene in the unit cell.
;
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     803
_refine_ls_number_reflns         16949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0389
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0823
_reflns_number_gt                12227
_reflns_number_total             16949
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3101787_si_003.cif
_cod_data_source_block           d:\chex_meo2-lut
_cod_database_code               4119208