Rhodium-Catalyzed Redox-Neutral Coupling of Phenidones with Alkynes
Fan, Zhoulong; Lu, Heng; Li, Wei; Geng, Kaijun; Zhang, Ao; Org. Biomol. Chem.  (2017) –; doi:10.1039/C7OB01271C

data_7155698
_publ_section_title
;
 Rhodium-Catalyzed Redox-Neutral Coupling of Phenidones with Alkynes
;
_journal_name_full               'Org. Biomol. Chem.'
_journal_paper_doi               10.1039/C7OB01271C
_journal_year                    2017
_chemical_formula_sum            'C23 H20 N2 O2.5'
_chemical_formula_weight         364.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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
;
2017-03-28 deposited with the CCDC.
2017-06-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.207(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.0516(14)
_cell_length_b                   8.6236(5)
_cell_length_c                   20.5558(10)
_cell_measurement_temperature    296(2)
_cell_volume                     4094.1(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0249
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15097
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    0.078
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM-PE'
_refine_diff_density_max         1.751
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       0.010(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   1.768
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3602
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.780
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.1177
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3849
_refine_ls_wR_factor_ref         0.4122
_reflns_number_gt                2662
_reflns_number_total             3602
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ob01271c2.cif
_cod_data_source_block           2013296_0m
_cod_original_formula_sum        'C23 H20 N2 O2.50'
_cod_database_code               7155698