Pure phosphotriesters as versatile ligands in transition metal catalysis: efficient hydrosilylation of ketones and diethylzinc addition to aldehydes
Bouhachicha, M.; Ngo Ndimba, A.; Roisnel, T.; Lalli, C.; Argouarch, G.; New J. Chem. 41 (2017) 4767–4770; doi:10.1039/C7NJ00566K

data_7056233
_publ_section_title
;
 Pure phosphotriesters as versatile ligands in transition metal catalysis:
 efficient hydrosilylation of ketones and diethylzinc addition to
 aldehydes
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              4767
_journal_page_last               4770
_journal_paper_doi               10.1039/C7NJ00566K
_journal_volume                  41
_journal_year                    2017
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C36 H24 O8 P2'
_chemical_formula_sum            'C36 H24 O8 P2'
_chemical_formula_weight         646.49
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2017-01-11 deposited with the CCDC.
2017-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                63.248(2)
_cell_angle_beta                 75.096(2)
_cell_angle_gamma                88.790(2)
_cell_formula_units_Z            2
_cell_length_a                   11.0531(5)
_cell_length_b                   12.0593(6)
_cell_length_c                   12.8518(7)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.01
_cell_measurement_wavelength     0.71073
_cell_volume                     1469.31(13)
_computing_cell_refinement       'APEX3 (Bruker, 2015); SAINT (Bruker, 2014)'
_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics    'SXGRAPH (Farrugia, 1999), Mercury (CSD, 2014)'
_computing_publication_material  'CRYSCALC (T. Roisnel, local program, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SIR97 (ALtomare et al., 1999)'
_diffrn_ambient_temperature      150
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0408
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29375
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.524
_diffrn_reflns_theta_min         3.010
_exptl_absorpt_coefficient_mu    0.205
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.461
_exptl_crystal_description       prism
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     415
_refine_ls_number_reflns         6741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0349
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0502P)^2^+0.6014P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0894
_refine_ls_wR_factor_ref         0.0962
_reflns_number_gt                5591
_reflns_number_total             6741
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7nj00566k2.cif
_cod_data_source_block           GA301
_cod_database_code               7056233
_shelx_res_checksum              19286