An efficient asymmetric hydrophosphonylation of unsaturated amides catalyzed by rare-earth metal amides [(Me3Si)2N]3RE(μ-Cl)Li(THF)3 with phenoxy-functionalized chiral prolinols
Fei, Zenghui; Zeng, Chao; Lu, Chengrong; Zhao, Bei; Yao, Yingming; RSC Adv. 7 (2017) 19306–; doi:10.1039/C7RA00468K

data_7228755
_publ_section_title
;
 An efficient asymmetric hydrophosphonylation of unsaturated amides
 catalyzed by rare-earth metal amides [(Me3Si)2N]3RE(\m-Cl)Li(THF)3 with
 phenoxy-functionalized chiral prolinols
;
_journal_issue                   31
_journal_name_full               'RSC Adv.'
_journal_page_first              19306
_journal_paper_doi               10.1039/C7RA00468K
_journal_volume                  7
_journal_year                    2017
_chemical_formula_sum            'C84 H87 N2 O4 Sc'
_chemical_formula_weight         1233.52
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2017-01-10 deposited with the CCDC.
2017-03-13 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.546
_cell_length_b                   24.517
_cell_length_c                   27.817
_cell_measurement_reflns_used    39955
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.5049
_cell_measurement_theta_min      3.0017
_cell_volume                     9238.228
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini'
_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  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0845
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44528
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_T_max  0.9766
_exptl_absorpt_correction_T_min  0.9539
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.887
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             2632
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.03(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     832
_refine_ls_number_reflns         20922
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0554
_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^)+(0.0838P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1503
_refine_ls_wR_factor_ref         0.1600
_reflns_number_gt                17160
_reflns_number_total             20922
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ra00468k2.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        9237.9
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               7228755