Alternative Route Toward Nitrones: Experimental and Theoretical Findings.
Safin, Damir A.; Mitoraj, Mariusz P.; Babashkina, Maria G.; Kubisiak, Piotr; Robeyns, Koen; Filinchuk, Yaroslav; The Journal of organic chemistry 82 (2017) 1666–1675; doi:10.1021/acs.joc.6b02821

data_4032321
_publ_section_title
;
 Alternative Route Toward Nitrones: Experimental and Theoretical Findings.
;
_journal_issue                   3
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              1666
_journal_page_last               1675
_journal_paper_doi               10.1021/acs.joc.6b02821
_journal_volume                  82
_journal_year                    2017
_chemical_formula_moiety         'C11 H13 N3 O'
_chemical_formula_sum            'C11 H13 N3 O'
_chemical_formula_weight         203.24
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_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
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_atom_sites_solution_hydrogens   mixed
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_cell_angle_beta                 91.052(5)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   5.9648(3)
_cell_length_b                   34.2029(15)
_cell_length_c                   10.1737(6)
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_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      25.2260
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
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_computing_data_collection       MAR
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
;
_computing_molecular_graphics    'MERCURY (Macrae et al., 2008)'
_computing_publication_material
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'MERCURY (Macrae et al., 2008), Platon (Spek, 2009)'

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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      297(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'MAR345 image plate'
_diffrn_measurement_method       '192 images, \D\F 0.75\% '
_diffrn_radiation_monochromator  'Xenocs Fox3D mirror'
_diffrn_radiation_source         'Rigaku UltraX 18 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0238
_diffrn_reflns_av_unetI/netI     0.0350
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10586
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.158
_diffrn_reflns_theta_max         25.158
_diffrn_reflns_theta_min         3.112
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84092
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_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_description       rod
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 2544 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.4(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.087
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         6849
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.087
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0600
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+0.8315P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1579
_refine_ls_wR_factor_ref         0.1676
_reflns_Friedel_coverage         0.962
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.942
_reflns_number_gt                6026
_reflns_number_total             6849
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b02821_si_007.cif
_cod_data_source_block           7'
_cod_original_cell_volume        2075.25(19)
_cod_database_code               4032321
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   0.987
_shelx_res_checksum              16683
_shelx_hkl_checksum              34540