Effect of the Phosphoryl Substituent in the Linear Nitrone on the Spin Trapping of Superoxide Radical and the Stability of the Superoxide Adduct: Combined Experimental and Theoretical Studies
Yang-Ping Liu; Lan-Fen Wang; Zhou Nie; Yi-Qiong Ji; Yang Liu; Ke-Jian Liu; Qiu Tian; Journal of Organic Chemistry 71 (2006) 7753–7762; doi:10.1021/jo061204m

data_4021981
_publ_section_title
;
 Effect of the Phosphoryl Substituent in the Linear Nitrone on the
 Spin Trapping of Superoxide Radical and the Stability of the Superoxide
 Adduct: Combined Experimental and Theoretical Studies
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              7753
_journal_page_last               7762
_journal_paper_doi               10.1021/jo061204m
_journal_volume                  71
_journal_year                    2006
_chemical_formula_sum            'C14 H22 N O5 P'
_chemical_formula_weight         315.30
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 96.49(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2504(15)
_cell_length_b                   23.958(5)
_cell_length_c                   9.5680(19)
_cell_measurement_reflns_used    15144
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      1.70
_cell_volume                     1651.3(6)
_computing_cell_refinement       'Rapid auto(Rigaku 2001)'
_computing_data_collection       'Rapid auto(Rigaku 2001)'
_computing_data_reduction        'Rapid auto(Rigaku 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku raxis Rapid IP Area Detector'
_diffrn_measurement_method       '\w oscillation'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15144
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.70
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_T_max  0.9613
_exptl_absorpt_correction_T_min  0.8719
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   abscor
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3798
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0567
_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^)+(0.1078P)^2^+0.2226P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1676
_refine_ls_wR_factor_ref         0.1832
_reflns_number_gt                2694
_reflns_number_total             3798
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo061204msi20060612_093848.cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4021981