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_1512209
_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         'C24 H25 N3 O2 S'
_chemical_formula_sum            'C24 H25 N3 O2 S'
_chemical_formula_weight         419.53
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_symmetry_space_group_name_Hall  '-P 1'
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_cell_formula_units_Z            4
_cell_length_a                   10.1571(3)
_cell_length_b                   13.2750(3)
_cell_length_c                   17.2305(4)
_cell_measurement_reflns_used    19341
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      73.2282
_cell_measurement_theta_min      2.7677
_cell_volume                     2111.84(10)
_computing_cell_refinement
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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)
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_computing_data_collection
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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)
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_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 0.981
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
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_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31829
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_diffrn_reflns_theta_max         73.39
_diffrn_reflns_theta_min         2.77
_exptl_absorpt_coefficient_mu    1.567
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
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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)
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    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.2912
_exptl_crystal_size_mid          0.0946
_exptl_crystal_size_min          0.0395
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
_refine_ls_number_parameters     546
_refine_ls_number_reflns         8351
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0507P)^2^+0.9477P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1049
_reflns_number_gt                7665
_reflns_number_total             8351
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol4016892_si_002.cif
_cod_data_source_block           2a
_cod_original_cell_volume        2111.83(9)
_cod_database_code               1512209