Iron-Catalyzed Direct Olefin Diazidation via Peroxyester Activation Promoted by Nitrogen-Based Ligands.
Shen, Shou-Jie; Zhu, Cheng-Liang; Lu, Deng-Fu; Xu, Hao; ACS catalysis 8 (2018) 4473–4482; doi:10.1021/acscatal.8b00821

data_4515601
_publ_section_title
;
 Iron-Catalyzed Direct Olefin Diazidation via Peroxyester Activation
 Promoted by Nitrogen-Based Ligands.
;
_journal_issue                   5
_journal_name_full               'ACS catalysis'
_journal_page_first              4473
_journal_page_last               4482
_journal_paper_doi               10.1021/acscatal.8b00821
_journal_volume                  8
_journal_year                    2018
_chemical_formula_sum            'C10 H12 Fe N11 O'
_chemical_formula_weight         358.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 106.559(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.820(7)
_cell_length_b                   12.675(7)
_cell_length_c                   11.662(7)
_cell_measurement_reflns_used    7928
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      2.27
_cell_volume                     1533.0(16)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0963
_diffrn_reflns_av_unetI/netI     0.0555
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            29170
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         2.266
_exptl_absorpt_coefficient_mu    1.007
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       blocklike
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.182
_exptl_crystal_size_mid          0.117
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.631
_refine_diff_density_min         -0.707
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.794
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         3144
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.793
_refine_ls_R_factor_all          0.1335
_refine_ls_R_factor_gt           0.0919
_refine_ls_shift/su_max          0.021
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1890P)^2^+17.8480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2621
_refine_ls_wR_factor_ref         0.3029
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2169
_reflns_number_total             3144
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b00821_si_002.cif
_cod_data_source_block           HX3
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4515601
_shelx_estimated_absorpt_t_min   0.838
_shelx_estimated_absorpt_t_max   0.910
_shelxl_version_number           2013-3
_shelx_res_checksum              14862
_shelx_hkl_checksum              19831