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_1554538
_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         'C27 H21 N2 O P'
_chemical_formula_sum            'C27 H21 N2 O P'
_chemical_formula_weight         420.43
_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'
_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                90
_cell_angle_beta                 90.13(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.429(3)
_cell_length_b                   10.415(2)
_cell_length_c                   37.841(8)
_cell_measurement_reflns_used    500
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.0
_cell_measurement_theta_min      3.5
_cell_volume                     4898.4(18)
_computing_cell_refinement       'iMosflm (Battye et al., 2011)'
_computing_data_collection       'Marccd (Doyle, 2011)'
_computing_data_reduction        iMosflm
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2015)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.956
_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  0.1035
_diffrn_reflns_av_unetI/netI     0.0866
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            46720
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        35.279
_diffrn_reflns_theta_max         38.468
_diffrn_reflns_theta_min         3.436
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_T_max  0.910
_exptl_absorpt_correction_T_min  0.880
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Scala (Evans, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.140
_exptl_crystal_description       prism
_exptl_crystal_F_000             1760
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.540
_refine_diff_density_rms         0.071
_refine_ls_extinction_coef       0.0062(5)
_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
_refine_ls_number_parameters     560
_refine_ls_number_reflns         10579
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0717
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0756P)^2^+P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1369
_refine_ls_wR_factor_ref         0.1567
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8072
_reflns_number_total             10579
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8qo01214h2.cif
_cod_data_source_block           11c
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1554538
_shelx_estimated_absorpt_t_min   0.886
_shelx_estimated_absorpt_t_max   0.912
_platon_squeeze_void_probe_radius 1.20
_shelxl_version_number           2014/6
_shelx_res_checksum              41052
_shelx_hkl_checksum              60871
_shelx_fab_checksum              77728