Facile C-N Cleavage in a Series of Bridged Lactams
Yao Lei; Aaron D. Wrobleski; Jennifer E. Golden; Douglas R. Powell; Jeffrey Aubé; Journal of the American Chemical Society 127 (2005) 4552–4553; doi:10.1021/ja050214m

data_4111593
_publ_contact_author
; 
   Prof. Jeffrey Aub\'e 
   Department of Medicinal Chemistry -- University of Kansas 
   Malott Hall 
   1251 Wescoe Hall Dr, Rm 4070 
   Lawrence, KS  66045-7582  USA 
;
_publ_contact_author_email       jaube@ku.edu
_publ_contact_author_fax         1(785)8645326
_publ_contact_author_phone       1(785)8644496
_publ_section_title
;
 Facile C-N Cleavage in a Series of Bridged Lactams
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4552
_journal_page_last               4553
_journal_paper_doi               10.1021/ja050214m
_journal_volume                  127
_journal_year                    2005
_chemical_formula_moiety         'C35 H35 Br2 N O6'
_chemical_formula_sum            'C35 H35 Br2 N O6'
_chemical_formula_weight         725.46
_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           SHELXL-97
_cell_angle_alpha                104.083(2)
_cell_angle_beta                 107.557(2)
_cell_angle_gamma                95.816(2)
_cell_formula_units_Z            2
_cell_length_a                   10.2457(8)
_cell_length_b                   12.9259(11)
_cell_length_c                   12.9628(10)
_cell_measurement_reflns_used    4553
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.92
_cell_measurement_theta_min      2.71
_cell_volume                     1559.0(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  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\w scan frames'
_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  0.0264
_diffrn_reflns_av_sigmaI/netI    0.0709
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9747
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        nil
_exptl_absorpt_coefficient_mu    2.648
_exptl_absorpt_correction_T_max  0.7777
_exptl_absorpt_correction_T_min  0.5243
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, 2000'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_density_meas      0
_exptl_crystal_description       prism
_exptl_crystal_F_000             740
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.907
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         7939
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.907
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0340P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                5438
_reflns_number_total             7939
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja050214msi20050112_055956_1.cif
_cod_data_source_block           SI-Q
_cod_database_code               4111593