Rhodium-Catalyzed [2 + 2 + 2] Cycloaddition of Alkenyl Isocyanates and Alkynes
Robert T. Yu; Tomislav Rovis; Journal of the American Chemical Society 128 (2006) 2782–2783; doi:10.1021/ja057803c

data_4110436
_publ_section_title
;
 Rhodium-Catalyzed [2 + 2 + 2] Cycloaddition of Alkenyl Isocyanates and
 Alkynes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2782
_journal_page_last               2783
_journal_paper_doi               10.1021/ja057803c
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C20 H19 N O'
_chemical_formula_weight         289.36
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 103.175(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.656(2)
_cell_length_b                   10.634(2)
_cell_length_c                   15.602(4)
_cell_measurement_temperature    298(2)
_cell_volume                     1559.9(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0845
_diffrn_reflns_av_sigmaI/netI    0.0629
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5581
_diffrn_reflns_theta_full        17.99
_diffrn_reflns_theta_max         17.99
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    0.075
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_F_000             616
_refine_diff_density_max         0.174
_refine_diff_density_min         -0.158
_refine_diff_density_rms         0.033
_refine_ls_extinction_coef       0.0008(13)
_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   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         1077
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0504
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+1.4569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1195
_refine_ls_wR_factor_ref         0.1404
_reflns_number_gt                720
_reflns_number_total             1077
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja057803csi20051129_071057.cif
_cod_data_source_block           rovis11m
_cod_database_code               4110436