Synthesis and Applications of Unquaternized C-Bound Boron Enolates.
Ng, Elvis Wang Hei; Low, Kam-Hung; Chiu, Pauline; Journal of the American Chemical Society 140 (2018) 3537–3541; doi:10.1021/jacs.8b00614

data_4132034
_publ_section_title
;
 Synthesis and Applications of Unquaternized C-Bound Boron Enolates.
;
_journal_issue                   10
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3537
_journal_page_last               3541
_journal_paper_doi               10.1021/jacs.8b00614
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C13 H24 B N O4'
_chemical_formula_sum            'C13 H24 B N O4'
_chemical_formula_weight         269.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.450(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.1648(3)
_cell_length_b                   16.1293(6)
_cell_length_c                   11.1095(4)
_cell_measurement_reflns_used    228
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45
_cell_measurement_theta_min      3
_cell_volume                     1447.16(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX3 v2015.5-2 (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT v8.34A (Bruker-AXS, 2007)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.24
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker D8 VENTURE FIXED-CHI PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10135
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        66.581
_diffrn_reflns_theta_max         66.581
_diffrn_reflns_theta_min         4.869
_diffrn_source                   'I\mS HB micro-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_T_max  0.5742
_exptl_absorpt_correction_T_min  0.0494
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5 (Sheldrick, 2014)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             584
_exptl_crystal_size_max          1.052
_exptl_crystal_size_mid          0.402
_exptl_crystal_size_min          0.206
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.525
_refine_diff_density_rms         0.110
_refine_ls_extinction_coef       0.0034(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2515
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0667
_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^)+(0.1568P)^2^+1.0091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2004
_refine_ls_wR_factor_ref         0.2289
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2037
_reflns_number_total             2515
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b00614_si_001.cif
_cod_data_source_block           cu_CHEM0222
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4132034
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.517
_shelx_estimated_absorpt_t_max   0.865
_shelx_res_checksum              22947
_shelx_hkl_checksum              34156