Irradiation of Imine-Group VI Carbene Complexes in the Presence of Alkynes: A Theoretical and Experimental Study
Pedro J. Campos; Diego Sampedro; Miguel A. Rodríguez; Journal of Organic Chemistry 68 (2003) 4674–4683; doi:10.1021/jo0343073

data_4022440
_publ_section_title
;
 Irradiation of Imine-Group VI Carbene Complexes in the Presence
 of Alkynes: A Theoretical and Experimental Study
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              4674
_journal_page_last               4683
_journal_paper_doi               10.1021/jo0343073
_journal_volume                  68
_journal_year                    2003
_chemical_formula_sum            'C20 H13 Cr N O5'
_chemical_formula_weight         399.31
_chemical_name_systematic
;
 ?
;
_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                 148.6590(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.8840(3)
_cell_length_b                   7.8230(2)
_cell_length_c                   23.5820(5)
_cell_measurement_reflns_used    11248
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     1907.96(7)
_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)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.1240
_diffrn_reflns_av_sigmaI/netI    0.0801
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            8408
_diffrn_reflns_theta_full        27.44
_diffrn_reflns_theta_max         27.44
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.629
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.403
_refine_diff_density_min         -1.511
_refine_diff_density_rms         0.388
_refine_ls_extinction_coef       0.255(12)
_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   1.510
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         4255
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.510
_refine_ls_R_factor_all          0.1363
_refine_ls_R_factor_gt           0.0873
_refine_ls_shift/su_max          5.509
_refine_ls_shift/su_mean         0.109
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0879P)^2^+0.2346P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1713
_refine_ls_wR_factor_ref         0.2270
_reflns_number_gt                3067
_reflns_number_total             4255
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo0343073si20030308_055320.cif
_cod_data_source_block           JA034514K
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4022440