Gold-Catalyzed Reactivity Reversal of Indolizidinone-Tethered β-Amino Allenes Controlled by the Stereochemistry
Alcaide, Benito; Almendros, Pedro; Fernández, Israel; Martín-Montero, Raúl; Martínez-Peña, Francisco; Ruiz, M. Pilar; Torres, M. Rosario; ACS Catalysis 5 (2015) 4842–; doi:10.1021/acscatal.5b01061

data_4513439
_publ_section_title
;
 Gold-Catalyzed Reactivity Reversal of Indolizidinone-Tethered \b-Amino
 Allenes Controlled by the Stereochemistry
;
_journal_issue                   8
_journal_name_full               'ACS Catalysis'
_journal_page_first              4842
_journal_paper_doi               10.1021/acscatal.5b01061
_journal_volume                  5
_journal_year                    2015
_chemical_absolute_configuration syn
_chemical_formula_sum            'C54 H47 N4 O7'
_chemical_formula_weight         863.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.3766(18)
_cell_length_b                   16.424(2)
_cell_length_c                   28.578(4)
_cell_measurement_reflns_used    2879
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      17.63
_cell_measurement_theta_min      2.18
_cell_volume                     5809.1(14)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1194
_diffrn_reflns_av_sigmaI/netI    0.2502
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            44355
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    0.066
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    0.988
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_platon_squeeze_details
;
The final refinement show high values of residual non-modelled 
 electronic density.Therefore, the Squeeze program was used to 
 remove its contribution to the overal intensity data.An 
 improvement was observed in all refinement parameters and residual
 when this procedure is applied   
;
_refine_diff_density_max         0.340
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.075
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         10220
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1916
_refine_ls_R_factor_gt           0.0820
_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^)+(0.0440P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1624
_refine_ls_wR_factor_ref         0.1748
_reflns_number_gt                3055
_reflns_number_total             10220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cs5b01061_si_003.cif
_cod_data_source_block           C54H47N4O7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 4513439--4513440.cif.
;
_cod_original_cell_volume        5809.2(15)
_cod_original_sg_symbol_H-M      P2(1)2(1)2(1)
_cod_database_code               4513439