Synthetic studies toward A-74528.
Hager, Anastasia; Mazunin, Dmitry; Mayer, Peter; Trauner, Dirk; Organic letters 13 (2011) 1386–1389; doi:10.1021/ol103117j

data_1501971
_publ_section_title
;
 Synthetic studies toward A-74528.
;
_journal_issue                   6
_journal_name_full               'Organic letters'
_journal_page_first              1386
_journal_page_last               1389
_journal_paper_doi               10.1021/ol103117j
_journal_volume                  13
_journal_year                    2011
_chemical_formula_moiety         'C17 H23 B O6'
_chemical_formula_sum            'C17 H23 B O6'
_chemical_formula_weight         334.172
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                C17H23BO6_no207_trauner
_audit_creation_date
;
'Tue Oct 27 06:47:57 2009'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             27-Oct-09
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.3923(8)
_cell_length_b                   10.6376(8)
_cell_length_c                   15.6535(14)
_cell_measurement_reflns_used    1773
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.2493
_cell_measurement_theta_min      4.2982
_cell_volume                     1730.5(2)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
;
_computing_structure_refinement
'SHELXL-97 (G. M. Sheldrick. University of G\"ottingen, 97-2 version)'
_computing_structure_solution
;
A. Altomare, M. C. Burla, M. Camalli, G. L. Cascarano, C. Giacovazzo, A.
Guagliardi, A. G. G. Moliterni, G. Polidori, R. Spagna: SIR97: a new tool for
crystal structure determination and refinement; J. Appl. Crystallogr. 1999,
32, 115-119.
;
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
  1 omega -103.00  -69.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.7619  179.0000  -90.0000 34

  2 omega   56.00  101.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9181  179.0000  150.0000 45

  3 omega   59.00   99.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9181  179.0000    0.0000 40

  4 omega  -32.00   90.00   1.0000   85.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9181    0.0000  150.0000 122

;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0631040293
_diffrn_orient_matrix_UB_12      -0.0145771748
_diffrn_orient_matrix_UB_13      0.0140878738
_diffrn_orient_matrix_UB_21      -0.0179989783
_diffrn_orient_matrix_UB_22      -0.0146380217
_diffrn_orient_matrix_UB_23      -0.0425706590
_diffrn_orient_matrix_UB_31      0.0186516312
_diffrn_orient_matrix_UB_32      -0.0634565476
_diffrn_orient_matrix_UB_33      0.0065274036
_diffrn_radiation_collimation    '0.5 mm collimator'
_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  0.0553
_diffrn_reflns_av_sigmaI/netI    0.0975
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7133
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         4.30
_diffrn_source_current           40_mA
_diffrn_source_power             2.00_kW
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           50_kV
_exptl_absorpt_coefficient_mu    0.095
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67012
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May  6 2009,17:20:42)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.28267(15)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.181
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   2.8(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.803
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         2003
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.803
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0454P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0922
_reflns_number_gt                1094
_reflns_number_total             2003
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol103117j_si_002.cif
_cod_data_source_block           no207
_cod_database_code               1501971