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_4022441
_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            'C19 H19 N O'
_chemical_formula_weight         277.35
_chemical_name_systematic
;                                                                               
 ?                                                                              
;
_space_group_IT_number           2
_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                89.4270(13)
_cell_angle_beta                 89.4150(14)
_cell_angle_gamma                62.973(3)
_cell_formula_units_Z            4
_cell_length_a                   8.8570(3)
_cell_length_b                   8.8560(4)
_cell_length_c                   22.9240(13)
_cell_measurement_temperature    293(2)
_cell_volume                     1601.62(13)
_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_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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            4517
_diffrn_reflns_theta_full        21.03
_diffrn_reflns_theta_max         31.03
_diffrn_reflns_theta_min         1.78
_exptl_absorpt_coefficient_mu    0.07
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             592
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.744
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     384
_refine_ls_number_reflns         3362
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.744
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.0828
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2133
_refine_ls_wR_factor_ref         0.2703
_reflns_number_gt                2241
_reflns_number_total             3362
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo0343073si20030308_055353.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_site_adp_type' tag value 'Uij' was replaced with 'Uani' value
43 times.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      'P -1          '
_cod_database_code               4022441