3,3-Diazidoenones – new types of highly reactive bis-azides. Preparation and synthetic transformations
Lemport, Pavel S.; Smolyar, Ivan V.; Khrustalev, Victor N.; Roznyatovsky, Vitaly A.; Popov, Alexander V.; Kobelevskaya, Valentina A.; Rozentsveig, Igor B.; Nenajdenko, Valentine G.; Organic Chemistry Frontiers 6 (2019) 335–; doi:10.1039/C8QO01214H

data_1554537
_publ_section_title
;
 3,3-Diazidoenones -- new types of highly reactive bis-azides. Preparation
 and synthetic transformations
;
_journal_issue                   3
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              335
_journal_paper_doi               10.1039/C8QO01214H
_journal_volume                  6
_journal_year                    2019
_chemical_formula_moiety         'C17 H17 Br N4 O'
_chemical_formula_sum            'C17 H17 Br N4 O'
_chemical_formula_weight         373.25
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     difmap
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2018-11-09 deposited with the CCDC.
2018-12-10 downloaded from the CCDC.
;
_cell_angle_alpha                69.94(3)
_cell_angle_beta                 83.57(3)
_cell_angle_gamma                89.74(3)
_cell_formula_units_Z            2
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_cell_measurement_reflns_used    600
_cell_measurement_temperature    100(2)
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_cell_measurement_theta_min      2.2
_cell_volume                     806.7(3)
_computing_cell_refinement       'iMosflm (Battye et al., 2011)'
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_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.898
_diffrn_measurement_device_type  'Rayonix SX165 CCD'
_diffrn_measurement_method       '/f scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.96260
_diffrn_reflns_av_R_equivalents  0.1002
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_diffrn_reflns_theta_min         2.239
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            'pale yellow'
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_exptl_crystal_description       prism
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.35
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_refine_ls_extinction_coef       0.009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         3237
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0871
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_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^)+(0.0278P)^2^+0.55P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1321
_refine_ls_wR_factor_ref         0.1567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2399
_reflns_number_total             3237
_reflns_threshold_expression     'I > 2\s(I)'
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_shelx_estimated_absorpt_t_min   0.783
_shelx_estimated_absorpt_t_max   0.917
_shelxl_version_number           2014/6
_shelx_res_checksum              62466
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