Effects of Solvent and Residual Water on Enhancing the Reactivity of Six-Membered Silyloxyallyl Cations toward Nucleophilic Addition.
Malone, Joshua A.; Cleveland, Alexander H.; Fronczek, Frank R.; Kartika, Rendy; Organic letters 18 (2016) 4408–4411; doi:10.1021/acs.orglett.6b02194

data_1555719
_publ_section_title
;
 Effects of Solvent and Residual Water on Enhancing the Reactivity of
 Six-Membered Silyloxyallyl Cations toward Nucleophilic Addition.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              4408
_journal_page_last               4411
_journal_paper_doi               10.1021/acs.orglett.6b02194
_journal_volume                  18
_journal_year                    2016
_chemical_formula_moiety         'C21 H30 Br N O Si'
_chemical_formula_sum            'C21 H30 Br N O Si'
_chemical_formula_weight         420.46
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           Monoclinic'
_symmetry_space_group_name_H-M   'P 1 21/n 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
_cell_angle_beta                 113.855(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.2375(6)
_cell_length_b                   14.2198(8)
_cell_length_c                   13.0699(6)
_cell_measurement_reflns_used    9964
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      34.46
_cell_measurement_theta_min      2.86
_cell_volume                     2080.06(19)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX 3'
_computing_data_reduction        'Bruker SAINT'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(5)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Kappa APEX-II DUO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'TRIUMPH curved graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0325
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46270
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         35.00
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    2.043
_exptl_absorpt_correction_T_max  0.7227
_exptl_absorpt_correction_T_min  0.6459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2004)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate fragment'
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.29
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_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.793
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_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         9109
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_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0329P)^2^+0.4396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
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_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ol6b02194_si_002.cif
_cod_data_source_block           Malone1
_cod_original_cell_volume        2080.06(18)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1555719