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

data_1501972
_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         'C15 H14 Br N O3'
_chemical_formula_sum            'C15 H14 Br N O3'
_chemical_formula_weight         336.181
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                C15H14BrNO3_no181_trauner
_audit_creation_date
;
'Thu Sep 24 09:57:00 2009'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             24-Sep-09
_cell_angle_alpha                88.983(3)
_cell_angle_beta                 84.074(3)
_cell_angle_gamma                83.609(3)
_cell_formula_units_Z            2
_cell_length_a                   7.8896(3)
_cell_length_b                   9.0992(3)
_cell_length_c                   9.4428(4)
_cell_measurement_reflns_used    3355
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.2445
_cell_measurement_theta_min      4.3294
_cell_volume                     670.06(4)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -32.00   52.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.8087   77.0000   60.0000 84

  2 omega   20.00   52.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.8087   77.0000  -60.0000 32

  3 omega  -53.00   49.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.8087   77.0000   30.0000 102

  4 omega  -12.00   77.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9650   77.0000  -60.0000 89

  5 omega  -12.00   87.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.9650   77.0000 -180.0000 99

;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       omega-scans
_diffrn_orient_matrix_UB_11      -0.0024035172
_diffrn_orient_matrix_UB_12      -0.0671854765
_diffrn_orient_matrix_UB_13      -0.0363112170
_diffrn_orient_matrix_UB_21      0.0881069095
_diffrn_orient_matrix_UB_22      -0.0195291463
_diffrn_orient_matrix_UB_23      0.0073881820
_diffrn_orient_matrix_UB_31      -0.0219854308
_diffrn_orient_matrix_UB_32      -0.0354080627
_diffrn_orient_matrix_UB_33      0.0657698723
_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  0.0218
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4733
_diffrn_reflns_theta_full        26.33
_diffrn_reflns_theta_max         26.33
_diffrn_reflns_theta_min         4.34
_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    3.074
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78568
_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    1.66627(10)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         2708
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0256
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0328P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0582
_refine_ls_wR_factor_ref         0.0588
_reflns_number_gt                2275
_reflns_number_total             2708
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol103117j_si_002.cif
_cod_data_source_block           no181
_cod_database_code               1501972