Phosphine-Promoted [4 + 3] Annulation of Allenoate with Aziridines for Synthesis of Tetrahydroazepines: Phosphine-Dependent [3 + 3] and [4 + 3] Pathways.
Liu, Honglei; Lin, Yan; Zhao, Yan; Xiao, Miaoren; Zhou, Leijie; Wang, Qijun; Zhang, Cheng; Wang, Dongqi; Kwon, Ohyun; Guo, Hongchao; RSC advances 9 (2019) 1214–1221; doi:10.1039/C8RA09852B

data_7232151
_publ_section_title
;
 Phosphine-Promoted [4 + 3] Annulation of Allenoate with Aziridines for
 Synthesis of Tetrahydroazepines: Phosphine-Dependent [3 + 3] and [4 + 3]
 Pathways.
;
_journal_issue                   3
_journal_name_full               'RSC advances'
_journal_page_first              1214
_journal_page_last               1221
_journal_paper_doi               10.1039/C8RA09852B
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C24 H26 N2 O8 S'
_chemical_formula_sum            'C24 H26 N2 O8 S'
_chemical_formula_weight         502.53
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-09-22 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;
_cell_angle_alpha                104.454(3)
_cell_angle_beta                 109.130(3)
_cell_angle_gamma                91.112(4)
_cell_formula_units_Z            2
_cell_length_a                   10.136(3)
_cell_length_b                   10.925(3)
_cell_length_c                   11.309(3)
_cell_measurement_reflns_used    5339
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.59
_cell_measurement_theta_min      3.85
_cell_volume                     1138.7(6)
_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-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0368
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15887
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         29.94
_diffrn_reflns_theta_min         3.85
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  0.9941
_exptl_absorpt_correction_T_min  0.9676
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Bruker)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.428
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     420
_refine_ls_number_reflns         6342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0386
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0457P)^2^+0.4056P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0926
_refine_ls_wR_factor_ref         0.1001
_reflns_number_gt                5084
_reflns_number_total             6342
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c8ra09852b2.cif
_cod_data_source_block           Sa4500a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7232151.cif.
;
_cod_original_cell_volume        1138.6(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7232151