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_4107690
_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         'C19 H21 N O4 S'
_chemical_formula_sum            'C19 H21 N O4 S'
_chemical_formula_weight         359.43
_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                100.181(1)
_cell_angle_beta                 98.924(1)
_cell_angle_gamma                99.436(1)
_cell_formula_units_Z            2
_cell_length_a                   7.3392(2)
_cell_length_b                   9.7040(2)
_cell_length_c                   12.7562(3)
_cell_measurement_reflns_used    3413
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      65.54
_cell_measurement_theta_min      8.38
_cell_volume                     866.09(4)
_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 0.710
_diffrn_measured_fraction_theta_max 0.710
_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  0.0125
_diffrn_reflns_av_sigmaI/netI    0.0161
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4246
_diffrn_reflns_theta_full        66.18
_diffrn_reflns_theta_max         66.18
_diffrn_reflns_theta_min         8.38
_exptl_absorpt_coefficient_mu    1.866
_exptl_absorpt_correction_T_max  0.7300
_exptl_absorpt_correction_T_min  0.4974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_description       prism
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.197
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         2161
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0334
_refine_ls_R_factor_gt           0.0328
_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^)+(0.0569P)^2^+0.4000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0918
_reflns_number_gt                2113
_reflns_number_total             2161
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja7111788-file003_3.cif
_cod_data_source_block           art3_066s
_cod_database_code               4107690