N,O-Nucleosides from Ene Reactions of Nitrosocarbonyl Intermediates with the 3-Methyl-2-buten-1-ol
Paolo Quadrelli; Mariella Mella; Serena Carosso; Bruna Bovio; Journal of Organic Chemistry 78 (2013) 516–526; doi:10.1021/jo302346a

data_4027855
_publ_section_title
;
 N,O-Nucleosides from Ene Reactions of Nitrosocarbonyl Intermediates with
 the 3-Methyl-2-buten-1-ol
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              516
_journal_page_last               526
_journal_paper_doi               10.1021/jo302346a
_journal_volume                  78
_journal_year                    2013
_chemical_compound_source        'prof.Paolo Quadrelli'
_chemical_formula_moiety         'C15 H21 N O3'
_chemical_formula_sum            'C15 H21 N O3'
_chemical_formula_weight         263.33
_chemical_name_systematic
N-mesitoyl-3,3-dimethyl-5-hydroxyl-isoxazolidine
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-93
_cell_angle_alpha                90.00
_cell_angle_beta                 104.26(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   8.551(1)
_cell_length_b                   21.374(4)
_cell_length_c                   17.241(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      7
_cell_volume                     3054.0(8)
_computing_cell_refinement       'CAD4 (Enraf Nonius, 1992)'
_computing_data_collection       'CAD4 (Enraf Nonius, 1992)'
_computing_data_reduction        'CAD4 (Enraf Nonius, 1992)'
_computing_molecular_graphics    'Ortep, (Johnson, 1965)'
_computing_structure_refinement  'Shelxl-93 (Sheldrick, 2008)'
_computing_structure_solution    'Shelxl-93 (sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710738
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_theta_full        30.0
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  240
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.886
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.145
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.83
_exptl_crystal_size_mid          0.77
_exptl_crystal_size_min          0.71
_refine_diff_density_max         0.19
_refine_diff_density_min         -0.14
_refine_diff_density_rms         0.1
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         4492
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0482
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0962P)^2^+0.34P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1121
_reflns_number_gt                4492
_reflns_number_observed          8807
_reflns_number_total             8865
_reflns_threshold_expression     >2s(I)
_cod_data_source_file            jo302346a_si_001.cif
_cod_data_source_block           cif11Bd
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_refinement_flags' value 'd' changed to 'D' according to
the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (80 times).

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4027855