Catalytic Metallonitrene/Alkyne Metathesis: A Powerful Cascade Process for the Synthesis of Nitrogen-Containing Molecules
Aaron R. Thornton; Simon B. Blakey; Journal of the American Chemical Society 130 (2008) 5020–5021; doi:10.1021/ja7111788

data_4107689
_publ_section_title
;
 Catalytic Metallonitrene/Alkyne Metathesis: A Powerful Cascade Process
 for the Synthesis of Nitrogen-Containing Molecules
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5020
_journal_page_last               5021
_journal_paper_doi               10.1021/ja7111788
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C10 H17 N O4 S'
_chemical_formula_sum            'C10 H17 N O4 S'
_chemical_formula_weight         247.31
_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                 98.949(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.957(7)
_cell_length_b                   7.6891(17)
_cell_length_c                   11.327(2)
_cell_measurement_reflns_used    382
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      60.20
_cell_measurement_theta_min      7.02
_cell_volume                     2405.3(9)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.892
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1054
_diffrn_reflns_av_sigmaI/netI    0.0804
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3309
_diffrn_reflns_theta_full        55.96
_diffrn_reflns_theta_max         55.96
_diffrn_reflns_theta_min         5.97
_exptl_absorpt_coefficient_mu    2.418
_exptl_absorpt_correction_T_max  0.9646
_exptl_absorpt_correction_T_min  0.5832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       plate
_exptl_crystal_F_000             1056
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.734
_refine_diff_density_min         -1.000
_refine_diff_density_rms         0.157
_refine_ls_extinction_coef       0.0009(3)
_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   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         1405
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.2518
_refine_ls_R_factor_gt           0.1341
_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^)+(0.0500P)^2^+90.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2789
_refine_ls_wR_factor_ref         0.3531
_reflns_number_gt                669
_reflns_number_total             1405
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7111788-file003_2.cif
_cod_data_source_block           art2_158s
_cod_database_code               4107689