A catalytic multicomponent coupling reaction for the enantioselective synthesis of spiroacetals
Lara Cala; Abraham Mendoza; Francisco J. Fananas; Felix Rodriguez; Chem.Commun. 49 (2013) 2715–; doi:10.1039/c3cc00118k

data_7108995
_publ_section_title
;
 A catalytic multicomponent coupling reaction for the enantioselective
 synthesis of spiroacetals
;
_journal_name_full               Chem.Commun.
_journal_page_first              2715
_journal_paper_doi               10.1039/c3cc00118k
_journal_volume                  49
_journal_year                    2013
_chemical_absolute_configuration ad
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C25 H21 Br1 N2 O5'
_chemical_formula_sum            'C25 H21 Br N2 O5'
_chemical_formula_weight         509.35
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-06-26T13:46:36-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 113.493(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3280(3)
_cell_length_b                   8.9133(2)
_cell_length_c                   11.9526(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_measurement_wavelength     1.5418
_cell_volume                     1106.81(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 8.264
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1121554
_diffrn_orient_matrix_UB_12      0.1111992
_diffrn_orient_matrix_UB_13      -0.0278337
_diffrn_orient_matrix_UB_21      -0.008035
_diffrn_orient_matrix_UB_22      -0.0402772
_diffrn_orient_matrix_UB_23      0.1220298
_diffrn_orient_matrix_UB_31      0.0967025
_diffrn_orient_matrix_UB_32      0.1261245
_diffrn_orient_matrix_UB_33      0.0638021
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0123
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            4470
_diffrn_reflns_theta_full        70
_diffrn_reflns_theta_max         74.18
_diffrn_reflns_theta_min         4.03
_exptl_absorpt_coefficient_mu    2.878
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.70292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.048
_exptl_crystal_size_min          0.041
_refine_diff_density_max         0.188
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.04
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.011(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         3099
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0233
_refine_ls_R_factor_gt           0.0232
_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^)+(0.0370P)^2^+0.2412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0631
_reflns_number_gt                3077
_reflns_number_total             3099
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3cc00118k.txt
_cod_data_source_block           new_trans
_cod_database_code               7108995