Efficient Synthesis of Imino-methano Tröger Bases by Nitrene Insertions into C-N Bonds.
Pujari, Sandip A.; Guénée, Laure; Lacour, Jérôme; Organic letters 15 (2013) 3930–3933; doi:10.1021/ol4016892

data_1512210
_publ_section_title
;
 Efficient Synthesis of Imino-methano Tr\"oger Bases by Nitrene Insertions
 into C-N Bonds.
;
_journal_issue                   15
_journal_name_full               'Organic letters'
_journal_page_first              3930
_journal_page_last               3933
_journal_paper_doi               10.1021/ol4016892
_journal_volume                  15
_journal_year                    2013
_chemical_formula_moiety         'C23 H22 N4 O5 S'
_chemical_formula_sum            'C23 H22 N4 O5 S'
_chemical_formula_weight         466.51
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
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_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                 108.918(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.3235(6)
_cell_length_b                   12.3190(5)
_cell_length_c                   13.1555(6)
_cell_measurement_reflns_used    4588
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      28.0871
_cell_measurement_theta_min      2.9144
_cell_volume                     2195.92(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'Ortep 3 (Farrugia, 1997)'
_computing_publication_material  ShelX_Acta
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_detector_area_resol_mean 10.4679
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0247
_diffrn_reflns_av_unetI/netI     0.0324
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10760
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.12
_diffrn_reflns_theta_min         3.01
_exptl_absorpt_coefficient_mu    0.191
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.959
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.3009
_exptl_crystal_size_mid          0.2400
_exptl_crystal_size_min          0.1468
_refine_diff_density_max         0.268
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4540
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0421
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0432P)^2^+1.0307P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                3638
_reflns_number_total             4540
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol4016892_si_002.cif
_cod_data_source_block           8
_cod_original_cell_volume        2195.92(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1512210