Gold-catalyzed nitrene transfer to activated alkynes: formation of α,β-unsaturated amidines.
Li, Chaoqun; Zhang, Liming; Organic letters 13 (2011) 1738–1741; doi:10.1021/ol2002607

data_1502066
_publ_section_title
;
 Gold-catalyzed nitrene transfer to activated alkynes: formation of
 \a,\b-unsaturated amidines.
;
_journal_issue                   7
_journal_name_full               'Organic letters'
_journal_page_first              1738
_journal_page_last               1741
_journal_paper_doi               10.1021/ol2002607
_journal_volume                  13
_journal_year                    2011
_chemical_formula_sum            'C15 H17 N3 O6 S'
_chemical_formula_weight         367.38
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_symmetry_space_group_name_Hall  '-P 2yn'
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_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.2060(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.4246(3)
_cell_length_b                   5.53670(10)
_cell_length_c                   20.8373(4)
_cell_measurement_temperature    296(2)
_cell_volume                     1739.31(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega scan'
_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  0.0214
_diffrn_reflns_av_sigmaI/netI    0.0200
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            6243
_diffrn_reflns_theta_full        58.90
_diffrn_reflns_theta_max         58.90
_diffrn_reflns_theta_min         3.26
_exptl_absorpt_coefficient_mu    1.995
_exptl_absorpt_correction_T_max  0.752
_exptl_absorpt_correction_T_min  0.521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.403
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             768
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.516
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       0.0014(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   1.332
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         2287
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.439
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+1.5824P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1828
_refine_ls_wR_factor_ref         0.1857
_reflns_number_gt                2124
_reflns_number_total             2287
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol2002607_si_002.cif
_cod_data_source_block           w012111
_cod_depositor_comments
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The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'multi scan' changed to
'multi-scan' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      p2(1)/n
_cod_database_code               1502066