Palladium catalyzed asymmetric hydrophosphination of α,β- and α,β,γ,δ-unsaturated malonate esters - efficient control of reactivity, stereo- and regio-selectivity.
Yang, Xiang-Yuan; Gan, Jun Hao; Li, Yongxin; Pullarkat, Sumod A.; Leung, Pak-Hing; Dalton transactions (Cambridge, England : 2003) 44 (2015) 1258–1263; doi:10.1039/c4dt02673j

data_7033208
_publ_section_title
;
 Palladium catalyzed asymmetric hydrophosphination of \a,\b- and
 \a,\b,\g,\d-unsaturated malonate esters - efficient control of
 reactivity, stereo- and regio-selectivity.
;
_journal_issue                   3
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1258
_journal_page_last               1263
_journal_paper_doi               10.1039/c4dt02673j
_journal_volume                  44
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C28 H29 O5 P'
_chemical_formula_weight         476.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 103.361(9)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.751(2)
_cell_length_b                   5.8887(8)
_cell_length_c                   19.552(3)
_cell_measurement_reflns_used    1590
_cell_measurement_temperature    103.(2)
_cell_measurement_theta_max      23.3186
_cell_measurement_theta_min      2.4292
_cell_volume                     1204.3(3)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      103.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0856
_diffrn_reflns_av_unetI/netI     0.1399
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            20068
_diffrn_reflns_theta_full        31.22
_diffrn_reflns_theta_max         31.22
_diffrn_reflns_theta_min         3.21
_exptl_absorpt_coefficient_mu    0.152
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.420
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.477
_refine_ls_abs_structure_details
;
Flack x determined using 1521 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.07(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     309
_refine_ls_number_reflns         7734
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0648
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0327P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1236
_reflns_number_gt                5156
_reflns_number_total             7734
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4dt02673j2.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 7033206--7033209.cif.'
_cod_database_code               7033208
_shelx_res_checksum              38141