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_1512211
_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         'C26 H29 N3 O2 S'
_chemical_formula_sum            'C26 H29 N3 O2 S'
_chemical_formula_weight         447.58
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
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_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 105.1047(12)
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_cell_length_a                   11.01618(13)
_cell_length_b                   27.3276(3)
_cell_length_c                   8.12476(10)
_cell_measurement_reflns_used    11077
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      73.2020
_cell_measurement_theta_min      3.2150
_cell_volume                     2361.42(5)
_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_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 1.000
_diffrn_measured_fraction_theta_max 0.987
_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  0.0208
_diffrn_reflns_av_unetI/netI     0.0159
_diffrn_reflns_limit_h_max       13
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_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
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_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            17805
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_diffrn_reflns_theta_max         73.39
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    1.432
_exptl_absorpt_correction_T_max  0.894
_exptl_absorpt_correction_T_min  0.752
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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    1.259
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.3102
_exptl_crystal_size_mid          0.0934
_exptl_crystal_size_min          0.0882
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         4682
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0576P)^2^+0.6863P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                4370
_reflns_number_total             4682
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol4016892_si_002.cif
_cod_data_source_block           11a
_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_sg_symbol_H-M      'P 21/c'
_cod_database_code               1512211