Generation and intramolecular reactivity of acyl radicals from alkynylthiol esters under reducing tin-free conditions.
Benati, Luisa; Calestani, Gianluca; Leardini, Rino; Minozzi, Matteo; Nanni, Daniele; Spagnolo, Piero; Strazzari, Samantha; Organic letters 5 (2003) 1313–1316; doi:10.1021/ol034252r

data_1507285
_publ_section_title
;
 Generation and intramolecular reactivity of acyl radicals from
 alkynylthiol esters under reducing tin-free conditions.
;
_journal_issue                   8
_journal_name_full               'Organic letters'
_journal_page_first              1313
_journal_page_last               1316
_journal_paper_doi               10.1021/ol034252r
_journal_volume                  5
_journal_year                    2003
_chemical_formula_sum            'C21 H20 N2 O2 S'
_chemical_formula_weight         364.46
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00(0)
_cell_angle_beta                 90.00(0)
_cell_angle_gamma                90.00(0)
_cell_formula_units_Z            4.00
_cell_length_a                   15.107(2)
_cell_length_b                   6.180(1)
_cell_length_c                   19.739(3)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293
_cell_measurement_theta_max      37.8
_cell_measurement_theta_min      22.1
_cell_volume                     1842.9(5)
_computing_cell_refinement       'Belletti et al., 1993'
_computing_data_collection       'Belletti, Cantoni & Pasquinelli,1993'
_computing_data_reduction        'DIFAU (Belletti et al.)'
_computing_molecular_graphics    'ORTEP3.2 (Farrugia, 1997)'
_computing_publication_material  'PARST (Nardelli, 1983)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR97 (Altomare et al., 1998)'
_diffrn_ambient_temperature      293
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       omega/2theta
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         fine-focussealedtube
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0201
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            3496
_diffrn_reflns_theta_max         70.04
_diffrn_reflns_theta_min         4.48
_diffrn_standards_decay_%        0.1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.6984
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.978
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.3136
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             768.0
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.910
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.14(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.015
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3386
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.080
_refine_ls_restrained_S_obs      1.053
_refine_ls_R_factor_all          0.1000
_refine_ls_R_factor_gt           0.0882
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          -0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2031P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2615
_refine_ls_wR_factor_ref         0.2287
_reflns_number_gt                2821
_reflns_number_total             3496
_reflns_threshold_expression     '>2 sigma(I)'
_cod_data_source_file            ol034252rsi20030212_104953.cif
_cod_data_source_block           lb402
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      Pna21
_cod_original_formula_sum        'C21 H20 N2 O2 S1'
_cod_database_code               1507285