A Unified Approach to trans-Hydrindane Sesterterpenoids
Daniel T. Hog; Peter Mayer; Dirk Trauner; Journal of Organic Chemistry 77 (2012) 5838–5843; doi:10.1021/jo300726z

data_4027265
_publ_contact_author_address
;
Department Chemie
Ludwig-Maximilians Universit\"at
Butenandtstra\&se 5-13 (Haus F)
D-81377 M\"unchen
Bundesrepublik Deutschland
;
_publ_contact_author_email       dirk.trauner@cup.uni-muenchen.de
_publ_contact_author_fax         '+49 089-2180-77972'
_publ_contact_author_name        'Dirk Trauner'
_publ_section_title
;
 A Unified Approach to trans-Hydrindane Sesterterpenoids
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              5838
_journal_page_last               5843
_journal_paper_doi               10.1021/jo300726z
_journal_volume                  77
_journal_year                    2012
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C12 H18 O3'
_chemical_formula_sum            'C12 H18 O3'
_chemical_formula_weight         210.270
_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_author_name               'P. Mayer'
_audit_block_code                C12H18O3_oo024_trauner
_audit_creation_date
;
'Tue Feb 09 07:11:47 2010'
;
_audit_creation_method           'form98_non/compatible with shelxl97-2'
_audit_update_record             09-Feb-10
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2588(5)
_cell_length_b                   9.4467(5)
_cell_length_c                   12.5446(7)
_cell_measurement_reflns_used    3134
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.2424
_cell_measurement_theta_min      4.3033
_cell_volume                     1097.21(10)
_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
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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
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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      173(2)
_diffrn_detector_area_resol_mean 15.9809
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -93.00   13.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.2931  -77.0000  150.0000 106

  2 omega  -49.00   48.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2306  -65.0000  -90.0000 97

  3 omega   67.00   94.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2306  179.0000  -60.0000 27

  4 omega   -9.00   16.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2306   77.0000   30.0000 25

  5 omega   65.00   93.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2306   77.0000   30.0000 28

  6 omega   21.00   53.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2306  -77.0000   60.0000 32

  7 omega  -49.00   53.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2306  -77.0000   30.0000 102

;
_diffrn_measurement_device       'CCD camera on \k-goniostat'
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_diffrn_orient_matrix_UB_11      -0.0135156330
_diffrn_orient_matrix_UB_12      -0.0522887577
_diffrn_orient_matrix_UB_13      0.0394015233
_diffrn_orient_matrix_UB_21      0.0625750943
_diffrn_orient_matrix_UB_22      -0.0374678649
_diffrn_orient_matrix_UB_23      -0.0165033725
_diffrn_orient_matrix_UB_31      0.0422757067
_diffrn_orient_matrix_UB_32      0.0389383504
_diffrn_orient_matrix_UB_33      0.0370616614
_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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8113
_diffrn_reflns_theta_full        26.33
_diffrn_reflns_theta_max         26.33
_diffrn_reflns_theta_min         4.31
_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    0.090
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89301
_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    1.27292(12)
_exptl_crystal_description       block
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.166
_refine_diff_density_min         -0.136
_refine_diff_density_rms         0.030
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -3.1(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         1301
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.969
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0320
_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^)+(0.0500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0784
_reflns_number_gt                1051
_reflns_number_total             1301
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo300726z_si_001_1.cif
_cod_data_source_block           oo024
_cod_database_code               4027265