Indium-assisted aluminium-based stereoselective allylation of prostereogenic α, α-disubstituted cycloalkanones and imines
Reddy, Chennakesava; Srinivasarao, Arulananda Babu; Aslam, Nayyar Ahmad; RSC Advances  (2014) –; doi:10.1039/C4RA04293J

data_7217624
_publ_section_title
;
 Indium-assisted aluminium-based stereoselective allylation of
 prostereogenic \a, \a-disubstituted cycloalkanones and imines
;
_journal_name_full               'RSC Advances'
_journal_paper_doi               10.1039/C4RA04293J
_journal_year                    2014
_chemical_formula_moiety         'C19 H24 Cl2 O3'
_chemical_formula_sum            'C19 H24 Cl2 O3'
_chemical_formula_weight         371.28
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2014-01-03T23:53:55-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                61.212(2)
_cell_angle_beta                 66.057(2)
_cell_angle_gamma                71.403(3)
_cell_formula_units_Z            2
_cell_length_a                   9.5268(4)
_cell_length_b                   11.1801(6)
_cell_length_c                   11.2526(5)
_cell_measurement_reflns_used    4758
_cell_measurement_temperature    298
_cell_measurement_theta_max      24.485
_cell_measurement_theta_min      2.168
_cell_volume                     948.53(8)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
        J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
        J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
        SHELXL, G.M. Sheldrick, Acta Cryst.
        2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'MO K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11741
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.1
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        SADABS-2008/1 (Bruker,2008) was used for absorption correction.
        R(int) was 0.0472 before and 0.0388 after correction.
        The Ratio of minimum to maximum transmission is 0.9173.
        The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.3
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3336
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0697
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+0.3658P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1022
_refine_ls_wR_factor_ref         0.1171
_reflns_number_gt                2371
_reflns_number_total             3336
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra04293j2.cif
_cod_data_source_block           sci216_cr720a_0m
_cod_database_code               7217624