Synthesis of β-Lactams from a N-Rhenaimine: Effect of the Transition Metal on the Energetic Profile of the Staudinger Reaction
Eva Hevia; Julio Pérez; Víctor Riera; Daniel Miguel; Pablo Campomanes; M. Isabel Menéndez; Tomás L. Sordo; Santiago García-Granda; Journal of the American Chemical Society 125 (2003) 3706–3707; doi:10.1021/ja034070s

data_4113613
_publ_contact_author_address
;
Departamento de Quimica Organica e Inorganica/IUQOEM-Facultad de Quimica 
Universidad de Oviedo
C/ Julian Claveria s/n
33006 Oviedo  (ASTURIAS)
SPAIN
;
_publ_contact_author_email       japm@sauron.quimica.uniovi.es
_publ_contact_author_fax         +34-985-103446
_publ_contact_author_name        'Julio P\'erez'
_publ_contact_author_phone       +34-985-102985
_publ_section_title
;
 Synthesis of \b-Lactams from a N-Rhenaimine: Effect of the Transition
 Metal on the Energetic Profile of the Staudinger Reaction
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3706
_journal_page_last               3707
_journal_paper_doi               10.1021/ja034070s
_journal_volume                  125
_journal_year                    2003
_chemical_formula_moiety         'C40 H28 N3 O4 Re, C4 H8 O'
_chemical_formula_sum            'C44 H36 N3 O5 Re'
_chemical_formula_weight         872.97
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 100.2153(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.7859(1)
_cell_length_b                   19.0409(2)
_cell_length_c                   22.9624(2)
_cell_measurement_reflns_used    73218
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      70.076
_cell_measurement_theta_min      0.883
_cell_volume                     7222.87(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_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      293(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '95mm CCD camera on \k-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0581
_diffrn_reflns_av_sigmaI/netI    0.0922
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            73218
_diffrn_reflns_theta_full        69.79
_diffrn_reflns_theta_max         69.79
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    7.002
_exptl_absorpt_correction_T_max  0.568
_exptl_absorpt_correction_T_min  0.382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.606
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             3488
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.271
_refine_diff_density_min         -1.658
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         6768
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0402
_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^)+(0.0238P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1100
_reflns_number_gt                5442
_reflns_number_total             6768
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja034070ssi20030111_062838.cif
_cod_data_source_block           Compound_2_(eh2)
_cod_original_sg_symbol_Hall     '-C 2yc '
_cod_database_code               4113613