α-Organoelement Nitrones: Synthesis, Properties, and IR and13C NMR Spectral and X-ray Structural Characterization†
Voinov, Maxim A.; Shevelev, Tikhon G.; Rybalova, Tatyana V.; Gatilov, Yury V.; Pervukhina, Natalie V.; Burdukov, Aleksei B.; Grigor'ev, Igor A.; Organometallics 26 (2007) 1607–; doi:10.1021/om060883o

data_4072619
_publ_section_title
;
 \a-Organoelement Nitrones:&#x00A0; Synthesis, Properties, and IR and13C
 NMR Spectral and X-ray Structural Characterization&#x2020;
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1607
_journal_paper_doi               10.1021/om060883o
_journal_volume                  26
_journal_year                    2007
_chemical_formula_moiety         'C20 H25 N2 O2 P'
_chemical_formula_sum            'C20 H25 N2 O2 P'
_chemical_formula_weight         356.39
_chemical_melting_point          404
_chemical_name_systematic
; 
 1,2,2,5,5-Pentamethyl-4-diphenylphosphinoyl-2,5-dihydro-1H-
 imidazole-3-oxide 
;
_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                 90.994(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.4029(8)
_cell_length_b                   8.9187(5)
_cell_length_c                   17.7928(12)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      12.9
_cell_measurement_theta_min      11.5
_cell_volume                     1967.9(2)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\q 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  0.0152
_diffrn_reflns_av_sigmaI/netI    0.0358
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3637
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0.0162
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.154
_exptl_absorpt_correction_T_max  0.9797
_exptl_absorpt_correction_T_min  0.9394
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.203
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.297
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.0024(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         3468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.059
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0551P)^2^+0.5380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1104
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                2653
_reflns_number_total             3468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om060883osi20060926_012347.cif
_cod_data_source_block           compound_2e_Voinov
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4072619