A practical strategy for construction and regulation of multi-functional triazepinium salts via highly efficient I2-catalyzed cyclization
Liu, Lang; She, Mengyao; Zhang, Jun; Wang, Zhaohui; Liu, Hua; Tang, Mi; Liu, Ping; Zhang, Shengyong; Li, Jianli; Green Chemistry 22 (2020) 3111–3116; doi:10.1039/C9GC04328D

data_7240286
_publ_section_title
;
 A practical strategy for construction and regulation of multi-functional
 triazepinium salts via highly efficient I2-catalyzed cyclization
;
_journal_issue                   10
_journal_name_full               'Green Chemistry'
_journal_page_first              3111
_journal_page_last               3116
_journal_paper_doi               10.1039/C9GC04328D
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         'I, C20 H15 N6 O'
_chemical_formula_sum            'C20 H15 I N6 O'
_chemical_formula_weight         482.28
_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
_audit_creation_date             2019-01-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-08-02 deposited with the CCDC.	2020-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.054(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.0435(6)
_cell_length_b                   11.5711(10)
_cell_length_c                   27.338(2)
_cell_measurement_reflns_used    5200
_cell_measurement_temperature    293
_cell_measurement_theta_max      22.25
_cell_measurement_theta_min      2.85
_cell_volume                     2534.5(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_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  0.1080
_diffrn_reflns_av_unetI/netI     0.1021
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            26413
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.399
_diffrn_reflns_theta_min         2.542
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.281
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0718 before and 0.0593 after correction. The Ratio of minimum to maximum transmission is 0.8698. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_description       block
_exptl_crystal_F_000             952
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         6311
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1421
_refine_ls_R_factor_gt           0.0722
_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^)+(0.0780P)^2^+3.9012P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1699
_refine_ls_wR_factor_ref         0.1942
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3267
_reflns_number_total             6311
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9gc04328d2.cif
_cod_data_source_block           sust_2192_lx_0ma_sq
_cod_depositor_comments
;Adding full bibliography for 7240283--7240286.cif.

 Adding full bibliography for 7240283--7240286.cif.
;
_cod_database_code               7240286
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C9(H9), C10(H10), C11(H11), C12(H12), C15(H15), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              81238
_shelx_hkl_checksum              41211
_shelx_fab_checksum              36655
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'