Synthesis of functionalized cyclic boronates.
Altenhofer, Erich; Harmata, Michael; Organic letters 16 (2014) 3–5; doi:10.1021/ol4029918

data_1513547
_publ_section_title
;
 Synthesis of functionalized cyclic boronates.
;
_journal_issue                   1
_journal_name_full               'Organic letters'
_journal_page_first              3
_journal_page_last               5
_journal_paper_doi               10.1021/ol4029918
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C14 H22 O1, 0.5(H2 O)'
_chemical_formula_sum            'C14 H23 O1.5'
_chemical_formula_weight         215.32
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 107.998(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.5316(10)
_cell_length_b                   13.8442(5)
_cell_length_c                   8.1046(3)
_cell_measurement_reflns_used    2931
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      70.7
_cell_measurement_theta_min      3.8
_cell_volume                     2404.38(17)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2008)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'APEX2 (Bruker AXS, 2008)'
_computing_molecular_graphics    'X-SEED, Barbour, 2001'
_computing_publication_material  'CIFTAB (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEXII CCD on X8 Prospector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  'Incoatec Helios Cu multilayer'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_sigmaI/netI    0.0295
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            7291
_diffrn_reflns_theta_full        65.04
_diffrn_reflns_theta_max         65.04
_diffrn_reflns_theta_min         3.80
_diffrn_source                   'microfocus tube'
_diffrn_standards_decay_%        0.0
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.82
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Data were corrected for decay and absorption using the program SADABS 
 (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of
 G\"ottingen, Germany).
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Needle
_exptl_crystal_F_000             952
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         1994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0469P)^2^+3.7394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1153
_refine_ls_wR_factor_ref         0.1203
_reflns_number_gt                1685
_reflns_number_total             1994
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol4029918_si_002.cif
_cod_data_source_block           EA-8-74B
_cod_original_cell_volume        2404.38(16)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C14 H23 O1.50'
_cod_database_code               1513547