Ultra-Easy Access to NH2-Functionalized TSILs, Their Potential as Highly Volume-Efficient Electrophile Scavengers, and Insights into the Electronics of Girard's Reagent T, A Venerable Chemical Work Horse
Soutullo, Morgan D.; Odom, Carl I.; Salter, E. Alan; Stenson, Alexandra C.; Sykora, Richard E.; Wierzbicki, Andrzej; Davis, James H.; Journal of Combinatorial Chemistry 9 (2007) 571–; doi:10.1021/cc060151j

data_1505009
_publ_section_title
;
 Ultra-Easy Access to NH2-Functionalized TSILs, Their Potential as Highly
 Volume-Efficient Electrophile Scavengers, and Insights into the
 Electronics of Girard's Reagent T, A Venerable Chemical Work Horse
;
_journal_issue                   4
_journal_name_full               'Journal of Combinatorial Chemistry'
_journal_page_first              571
_journal_paper_doi               10.1021/cc060151j
_journal_volume                  9
_journal_year                    2007
_chemical_formula_moiety         'C24 H20 B, C9 H20 N3 O'
_chemical_formula_sum            'C33 H40 B N3 O'
_chemical_formula_weight         505.49
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.48(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.630(2)
_cell_length_b                   13.9808(15)
_cell_length_c                   12.999(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      11.52
_cell_measurement_theta_min      4.93
_cell_volume                     3021.3(9)
_computing_cell_refinement       'CAD4/PC v1.2'
_computing_data_collection       'CAD4/PC v1.2'
_computing_data_reduction        XCAD4PC
_computing_molecular_graphics    'SHELXP-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXCIF-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius CAD4'
_diffrn_measurement_method       'Th/2Th 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  0.0697
_diffrn_reflns_av_sigmaI/netI    0.2390
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3329
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         2.14
_diffrn_standards_interval_time  7200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.9730
_exptl_absorpt_correction_T_min  0.8672
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'North et al., 1968'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.700
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.152
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.0026(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.920
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         3148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.920
_refine_ls_R_factor_all          0.2422
_refine_ls_R_factor_gt           0.0511
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0399P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1019
_refine_ls_wR_factor_ref         0.1480
_reflns_number_gt                1113
_reflns_number_total             3148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cc060151jsi20070424_044351.cif
_cod_data_source_block           Girard3
_cod_original_cell_volume        3021.1(9)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1505009