Synthesis and Reactivity of 1-Allenyltriazenes.
Jeanbourquin, Loïc N; Scopelliti, Rosario; Fadaei Tirani, Farzaneh; Severin, Kay; Organic letters 19 (2017) 2070–2073; doi:10.1021/acs.orglett.7b00671

data_1545936
_publ_section_title
;
 Synthesis and Reactivity of 1-Allenyltriazenes.
;
_journal_issue                   8
_journal_name_full               'Organic letters'
_journal_page_first              2070
_journal_page_last               2073
_journal_paper_doi               10.1021/acs.orglett.7b00671
_journal_volume                  19
_journal_year                    2017
_chemical_formula_moiety         'C11 H21 N3'
_chemical_formula_sum            'C11 H21 N3'
_chemical_formula_weight         195.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 98.000(11)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   10.4021(10)
_cell_length_b                   11.1735(9)
_cell_length_c                   21.729(3)
_cell_measurement_reflns_used    2654
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      61.7870
_cell_measurement_theta_min      4.2760
_cell_volume                     2500.9(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1333
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -18.00  62.00   1.00   10.00    --    0.00  57.00-120.00   80
  2  \w    -62.00  23.00   1.00   10.00    --    0.00 -37.00  60.00   85
  3  \w    -87.00 -38.00   1.00   10.00    --    0.00 178.00-180.00   49
  4  \w     57.00  97.00   1.00   40.00    --   81.95-125.00-150.00   40
  5  \w     11.00 114.00   1.00   40.00    --   81.95 -77.00 -90.00  103
  6  \w      7.00 110.00   1.00   40.00    --   81.95 -30.00  90.00  103
  7  \w     52.00  97.00   1.00   40.00    --   81.95-125.00 -90.00   45
  8  \w     20.00 115.00   1.00   40.00    --   81.95 -77.00  30.00   95
  9  \w     70.00 151.00   1.00   40.00    --   81.95  30.00  90.00   81
 10  \w    108.00 141.00   1.00   40.00    --   81.95 125.00 120.00   33
 11  \w     68.00 147.00   1.00   40.00    --   81.95  45.00 -30.00   79
 12  \w    120.00 155.00   1.00   40.00    --   81.95  45.00-180.00   35
 13  \w     95.00 123.00   1.00   40.00    --   81.95-131.00  16.00   28
 14  \w    117.00 145.00   1.00   40.00    --   81.95 125.00-150.00   28
 15  \w     95.00 135.00   1.00   40.00    --   81.95 125.00   0.00   40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0459
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12845
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        62.177
_diffrn_reflns_theta_max         62.177
_diffrn_reflns_theta_min         4.109
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.487
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model.
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.037
_exptl_crystal_description       plate
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.711
_exptl_crystal_size_mid          0.589
_exptl_crystal_size_min          0.215
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         3883
_refine_ls_number_restraints     802
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1303
_refine_ls_R_factor_gt           0.0949
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1556P)^2^+1.4661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2668
_refine_ls_wR_factor_ref         0.3074
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2486
_reflns_number_total             3883
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b00671_si_002.cif
_cod_data_source_block           shelx
_cod_database_code               1545936
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              39515
_shelx_hkl_checksum              66923