Enantioselective O- and N-Nitroso Aldol Synthesis of Tin Enolates. Isolation of Three BINAP-Silver Complexes and Their Role in Regio- and Enantioselectivity
Norie Momiyama; Hisashi Yamamoto; Journal of the American Chemical Society 126 (2004) 5360–5361; doi:10.1021/ja039103i

data_4112531
_publ_section_title
;
 Enantioselective O- and N-Nitroso Aldol Synthesis of Tin Enolates.
 Isolation of Three BINAP-Silver Complexes and Their Role in Regio- and
 Enantioselectivity
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5360
_journal_page_last               5361
_journal_paper_doi               10.1021/ja039103i
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C89 H66 Ag Cl1.75 F0 O4 P4 S'
_chemical_formula_weight         1525.27
_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                   11.883(2)
_cell_length_b                   21.427(4)
_cell_length_c                   28.346(6)
_cell_measurement_temperature    103(2)
_cell_volume                     7217(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      103(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  0.0460
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            70489
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.516
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_F_000             3139
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.631
_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   0.022(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     915
_refine_ls_number_reflns         12751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.611
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^2^+2.0188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1092
_refine_ls_wR_factor_ref         0.1102
_reflns_number_gt                12386
_reflns_number_total             12751
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja039103isi20040121_010407.cif
_cod_data_source_block           momynus
_cod_original_cell_volume        7217(3)
_cod_database_code               4112531