Grignard Reagent-Mediated Conversion of an Acyl Nitroso-anthracene Cycloadduct to a Nitrone
Weibin Chen; Cynthia S. Day; S. Bruce King; Journal of Organic Chemistry 71 (2006) 9221–9224; doi:10.1021/jo0615192

data_4022102
_publ_contact_author_address
; 
Department of Chemistry 
Wake Forest University
Winston-Salem, N.C. 27109
U.S.A.
;
_publ_contact_author_email       kingsb@wfu.edu
_publ_contact_author_fax         '336 758 4656'
_publ_contact_author_name        'S. Bruce King'
_publ_contact_author_phone       '336 758 5774'
_publ_section_title
;
 Grignard Reagent-Mediated Conversion of an Acyl Nitroso-anthracene
 Cycloadduct to a Nitrone
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              9221
_journal_page_last               9224
_journal_paper_doi               10.1021/jo0615192
_journal_volume                  71
_journal_year                    2006
_chemical_formula_sum            'C38 H34 N2 O2'
_chemical_formula_weight         550.67
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                93.279(19)
_cell_angle_beta                 96.129(19)
_cell_angle_gamma                92.54(2)
_cell_formula_units_Z            2
_cell_length_a                   8.506(8)
_cell_length_b                   11.707(11)
_cell_length_c                   14.351(13)
_cell_measurement_reflns_used    485
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      18.149
_cell_measurement_theta_min      3.937
_cell_volume                     1417(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2844
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7933
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.92
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.079
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.263
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.759
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         7933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.759
_refine_ls_R_factor_all          0.1931
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0117P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.1210
_reflns_number_gt                2969
_reflns_number_total             7933
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo0615192si20060721_113645.cif
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_database_code               4022102