<i>rac</i>-(1<i>R</i>,11<i>S</i>,12<i>R</i>)-Ethyl 12-hydroxy-15-oxobicyclo[9.3.1]pentadecane-1-carboxylate
Fresu, Sonia; Schürmann, Markus; Preut, Hans; Eilbracht, Peter; Acta Crystallographica Section E 60 (2004) o22–o24; doi:10.1107/S160053680302717X

data_2203071
_publ_section_title
;
 <i>rac</i>-(1<i>R</i>,11<i>S</i>,12<i>R</i>)-Ethyl
 12-hydroxy-15-oxobicyclo[9.3.1]pentadecane-1-carboxylate
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o22
_journal_page_last               o24
_journal_paper_doi               10.1107/S160053680302717X
_journal_volume                  60
_journal_year                    2004
_chemical_formula_iupac          'C18 H30 O4'
_chemical_formula_moiety         'C18 H30 O4'
_chemical_formula_sum            'C18 H30 O4'
_chemical_formula_weight         310.42
_chemical_name_systematic
;Ethyl
 rac-(1R,11S,12R)-12-hydroxy-15-oxobicyclo[9.3.1]pentadecane-1-carboxylate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                68.0725(9)
_cell_angle_beta                 89.2421(9)
_cell_angle_gamma                65.8290(10)
_cell_formula_units_Z            4
_cell_length_a                   12.3829(3)
_cell_length_b                   12.8139(2)
_cell_length_c                   13.2413(3)
_cell_measurement_reflns_used    19813
_cell_measurement_temperature    291.0(10)
_cell_measurement_theta_max      27.53
_cell_measurement_theta_min      3.04
_cell_volume                     1753.78(7)
_computing_cell_refinement
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
DENZO & SCALEPACK
;
_computing_molecular_graphics    'SHETLXL-Plus (Sheldrick, 1991)'
_computing_publication_material
;
SHELXL97, PARST95 (Nardelli, 1995) and PLATON (Spek, 2001)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291.0(10)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
;
356 frames via \w-rotation (\D\w =1 \%) and two times 20 s per frame
(four sets at different \k angles)
;
_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  0.031
_diffrn_reflns_av_sigmaI/netI    0.1748
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19813
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.53
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.176
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.258
_refine_diff_density_min         -0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.861
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         7889
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.861
_refine_ls_R_factor_all          0.1879
_refine_ls_R_factor_gt           0.0435
_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^)+(0.0215P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0918
_reflns_number_gt                2673
_reflns_number_total             7889
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg6009.cif
_cod_data_source_block           I
_cod_database_code               2203071
_cod_database_fobs_code          2203071