Hydroboration Catalyzed by 1,2,4,3-Triazaphospholenes.
Tien, Chieh-Hung; Adams, Matt R.; Ferguson, Michael J.; Johnson, Erin R.; Speed, Alexander W. H.; Organic letters 19 (2017) 5565–5568; doi:10.1021/acs.orglett.7b02695

data_1547663
_publ_section_title
;
 Hydroboration Catalyzed by 1,2,4,3-Triazaphospholenes.
;
_journal_issue                   20
_journal_name_full               'Organic letters'
_journal_page_first              5565
_journal_page_last               5568
_journal_paper_doi               10.1021/acs.orglett.7b02695
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C23 H31 Br N3 P'
_chemical_formula_weight         460.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
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_cell_angle_gamma                105.0315(6)
_cell_formula_units_Z            4
_cell_length_a                   9.1345(4)
_cell_length_b                   14.6643(7)
_cell_length_c                   18.0325(8)
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_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      2.28
_cell_volume                     2313.62(18)
_computing_cell_refinement       'Bruker SAINT'
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_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
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_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
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_diffrn_reflns_limit_l_min       -23
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_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_max         27.574
_diffrn_reflns_theta_min         1.895
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_exptl_absorpt_correction_T_max  0.5982
_exptl_absorpt_correction_T_min  0.4348
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            colourless
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_exptl_crystal_description       block
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_exptl_crystal_size_mid          0.296
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         10603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0318
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+0.7509P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0795
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_reflns_number_gt                8601
_reflns_number_total             10603
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b02695_si_001.cif
_cod_data_source_block           dal1681
_cod_depositor_comments          'Adding full bibliography for 1547663.cif.'
_cod_database_code               1547663
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.576
_shelx_estimated_absorpt_t_max   0.830
_shelx_res_checksum              33443
_shelx_hkl_checksum              43075