Intermolecular nitroso Diels-Alder cycloaddition of alpha-acetoxynitroso derivatives in aqueous medium.
Calvet, Géraldine; Guillot, Régis; Blanchard, Nicolas; Kouklovsky, Cyrille; Organic & biomolecular chemistry 3 (2005) 4395–4401; doi:10.1039/b513397a

data_7151356
_publ_section_title
;
 Intermolecular nitroso Diels-Alder cycloaddition of
 alpha-acetoxynitroso derivatives in aqueous medium.
;
_journal_issue                   24
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              4395
_journal_page_last               4401
_journal_paper_doi               10.1039/b513397a
_journal_volume                  3
_journal_year                    2005
_chemical_formula_sum            'C16 H26 N2 O9'
_chemical_formula_weight         390.39
_chemical_name_common
;
acetic acid 5-(5-acetoxy-2,2-dimethyl-(1,3)dioxan-5-yl-ONN-
azoxy)-2,2-dimethyl-(1,3)dioxan-5-yl ester
;
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   10.6750(4)
_cell_length_b                   10.8521(5)
_cell_length_c                   33.5940(12)
_cell_measurement_temperature    293(2)
_cell_volume                     3891.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0230
_diffrn_reflns_av_sigmaI/netI    0.0367
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            7851
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.21
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.109
_exptl_absorpt_correction_T_max  0.985
_exptl_absorpt_correction_T_min  0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         4347
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.149
_refine_ls_shift/su_mean         0.019
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w==1/[\s^2^(Fo^2^)+(0.0681P)^2^+0.5549P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1383
_reflns_number_gt                2829
_reflns_number_total             4347
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b513397a.txt
_cod_data_source_block           azo
_cod_database_code               7151356