Asymmetric radical additions of trialkylboranes to 2H-azirine-3-carboxylates
Risberg, Erik; Fischer, Andreas; Somfai, Peter; Chemical Communications  (2004) 2088–2089; doi:10.1039/b408532a

data_7111400
_publ_section_title
;
 Asymmetric radical additions of trialkylboranes to
 2H-azirine-3-carboxylates
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              2088
_journal_page_last               2089
_journal_paper_doi               10.1039/b408532a
_journal_year                    2004
_chemical_compound_source        'Local laboratory'
_chemical_formula_moiety         'C15 H23 N2 O3 S'
_chemical_formula_sum            'C15 H23 N2 O3 S'
_chemical_formula_weight         311.43
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           maXus
_cell_angle_alpha                90.00
_cell_angle_beta                 91.273(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.7254(6)
_cell_length_b                   11.9768(9)
_cell_length_c                   24.980(2)
_cell_measurement_reflns_used    65
_cell_measurement_temperature    299
_cell_measurement_theta_max      15.61
_cell_measurement_theta_min      3.87
_cell_volume                     3208.0(4)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       KappaCCD
_computing_data_reduction
;
Denzo and Scalepack (Otwinowski & Minor, 1997)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      299
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength_id  all
_diffrn_reflns_av_R_equivalents  0.0490
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26285
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         4.51
_exptl_absorpt_coefficient_mu    0.214
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.332
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.05(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         8908
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0851
_refine_ls_R_factor_gt           0.0590
_refine_ls_shift/su_max          0.155
_refine_ls_shift/su_mean         0.007
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+2.6900P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1122
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                7055
_reflns_number_total             8908
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            b408532asup1.cif
_cod_data_source_block           compound_1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3208.1(3)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7111400