Azetidine-Borane Complexes: Synthesis, Reactivity, and Stereoselective Functionalization.
Andresini, Michael; De Angelis, Sonia; Uricchio, Antonella; Visaggio, Angelica; Romanazzi, Giuseppe; Ciriaco, Fulvio; Corriero, Nicola; Degennaro, Leonardo; Luisi, Renzo; The Journal of organic chemistry 83 (2018) 10221–10230; doi:10.1021/acs.joc.8b01441

data_4035121
_publ_section_title
;
 Azetidine-Borane Complexes: Synthesis, Reactivity, and Stereoselective
 Functionalization.
;
_journal_issue                   17
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              10221
_journal_page_last               10230
_journal_paper_doi               10.1021/acs.joc.8b01441
_journal_volume                  83
_journal_year                    2018
_chemical_formula_sum            'C11 H18 B N'
_chemical_formula_weight         175.07
_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   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 104.30(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.820(5)
_cell_length_b                   6.017(1)
_cell_length_c                   14.764(5)
_cell_measurement_reflns_used    130
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2
_cell_volume                     1103.6(6)
_computing_cell_refinement
'DIRAX (Duisenberg,1992; Duisenberg et al., 2000)'
_computing_data_collection       'COLLECT (Nonius, 2002)'
_computing_data_reduction        'EVAL (Nonius, 2002; Duisenberg et al., 2003)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SIR2014 (Burla et al., 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker-Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0911
_diffrn_reflns_av_unetI/netI     0.0626
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11147
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.509
_diffrn_reflns_theta_min         3.674
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.059
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS(Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.054
_exptl_crystal_description       block
_exptl_crystal_F_000             384
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.4793
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2521
_refine_ls_number_restraints     33
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0701
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1454P)^2^+0.0610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1986
_refine_ls_wR_factor_ref         0.2311
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1619
_reflns_number_total             2521
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo8b01441_si_001.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        1103.6(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4035121
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              91054
_shelx_hkl_checksum              27838