Decarboxylative Csp(3)-Csp(3) coupling for benzylation of unstable ketone enolates: synthesis of p-(acylethyl)phenols.
Wang, Sasa; Chen, Xinzheng; Ao, Qiaoqiao; Wang, Huifei; Zhai, Hongbin; Chemical communications (Cambridge, England) 52 (2016) 9454–9457; doi:10.1039/c6cc03835b

data_7124692
_publ_section_title
;
 Decarboxylative Csp(3)-Csp(3) coupling for benzylation of unstable ketone
 enolates: synthesis of p-(acylethyl)phenols.
;
_journal_issue                   60
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9454
_journal_page_last               9457
_journal_paper_doi               10.1039/c6cc03835b
_journal_volume                  52
_journal_year                    2016
_chemical_formula_sum            'C H N O S'
_chemical_formula_weight         75.09
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2016-06-17 deposited with the CCDC.
2016-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.130(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            26
_cell_length_a                   15.924(5)
_cell_length_b                   8.289(2)
_cell_length_c                   15.498(6)
_cell_measurement_temperature    566(2)
_cell_volume                     2019.7(11)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      566(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0861
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16179
_diffrn_reflns_theta_full        25.27
_diffrn_reflns_theta_max         25.27
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.768
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             988
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.075
_refine_ls_extinction_coef       0.37(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.754
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3567
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.754
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0802
_refine_ls_shift/su_max          0.061
_refine_ls_shift/su_mean         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2216
_refine_ls_wR_factor_ref         0.2515
_reflns_number_gt                2926
_reflns_number_total             3567
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc03835b2.cif
_cod_data_source_block           a
_cod_database_code               7124692