Radical Borylation/Cyclization Cascade of 1,6-Enynes for the Synthesis of Boron-Handled Hetero- and Carbocycles.
Ren, Shi-Chao; Zhang, Feng-Lian; Qi, Jing; Huang, Yun-Shuai; Xu, Ai-Qing; Yan, Hong-Yi; Wang, Yi-Feng; Journal of the American Chemical Society 139 (2017) 6050–6053; doi:10.1021/jacs.7b01889

data_4125939
_publ_section_title
;
 Radical Borylation/Cyclization Cascade of 1,6-Enynes for the Synthesis of
 Boron-Handled Hetero- and Carbocycles.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6050
_journal_page_last               6053
_journal_paper_doi               10.1021/jacs.7b01889
_journal_volume                  139
_journal_year                    2017
_chemical_formula_sum            'C26 H32 B N3 O4 S'
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_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
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_cell_angle_alpha                90
_cell_angle_beta                 97.673(2)
_cell_angle_gamma                90
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_cell_length_c                   16.1916(3)
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_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      71.2060
_cell_measurement_theta_min      4.0700
_cell_volume                     5383.00(16)
_computing_cell_refinement       'CrysAlisPro (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro (Rigaku OD, 2015)'
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_computing_molecular_graphics    'Ortep-3 (L. J. Farrugia, 2001)'
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_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      291(2)
_diffrn_detector_area_resol_mean 5.2169
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0262
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.993
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_diffrn_reflns_limit_h_min       -46
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_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14682
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.303
_diffrn_reflns_theta_min         4.069
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    1.353
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       block
_exptl_crystal_F_000             2096
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.230
_exptl_crystal_size_min          0.200
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_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     321
_refine_ls_number_reflns         5088
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0708
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0980P)^2^+5.7510P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1931
_refine_ls_wR_factor_ref         0.2084
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3896
_reflns_number_total             5088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            4b.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 4125939--4125941.cif.'
_cod_database_code               4125939
_shelx_estimated_absorpt_t_min   0.703
_shelx_estimated_absorpt_t_max   0.774
_shelxl_version_number           2013-4
_shelx_res_checksum              93551
_shelx_hkl_checksum              86737