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

data_1501970
_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         'C29 H28 O8'
_chemical_formula_sum            'C29 H28 O8'
_chemical_formula_weight         504.528
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_code                C29H28O8_oo110_trauner
_audit_creation_date
;
'Mon May 10 14:31:59 2010'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             10-May-10
_cell_angle_alpha                90.00
_cell_angle_beta                 113.387(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.0088(8)
_cell_length_b                   8.1117(3)
_cell_length_c                   18.6667(9)
_cell_measurement_reflns_used    3751
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.2500
_cell_measurement_theta_min      4.2026
_cell_volume                     2502.8(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
;
Sheldrick, G. M. (2008).
<i>Acta Cryst.</i> A<b>64</b>, 112--122.
;
_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      200(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   34.00   64.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2306  179.0000 -180.0000 30

  2 omega  -39.00   85.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2306    0.0000   90.0000 124

  3 omega   -4.00   77.00   1.0000   32.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2306   38.0000  -30.0000 81

;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
_diffrn_measurement_device_type  'Oxford XCalibur'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0042706129
_diffrn_orient_matrix_UB_12      -0.0244007311
_diffrn_orient_matrix_UB_13      0.0346045006
_diffrn_orient_matrix_UB_21      -0.0375184830
_diffrn_orient_matrix_UB_22      0.0420897621
_diffrn_orient_matrix_UB_23      -0.0125798061
_diffrn_orient_matrix_UB_31      -0.0203142685
_diffrn_orient_matrix_UB_32      -0.0726731882
_diffrn_orient_matrix_UB_33      -0.0188608424
_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  0.0228
_diffrn_reflns_av_sigmaI/netI    0.0544
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            9844
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         4.23
_diffrn_source_current           45_mA
_diffrn_source_power             2.48_kW
_diffrn_source_type              'Spellman generator'
_diffrn_source_voltage           55_kV
_exptl_absorpt_coefficient_mu    0.098
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96203
_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    1.33896(10)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.691
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.908
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.908
_refine_ls_R_factor_all          0.0808
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0810P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1247
_refine_ls_wR_factor_ref         0.1338
_reflns_number_gt                3021
_reflns_number_total             5051
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol103117j_si_002.cif
_cod_data_source_block           oo110
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1501970