Methyl <i>rac</i>-(1<i>S</i>*,11<i>R</i>*,12<i>S</i>*,14<i>S</i>*)-12-hydroxy-14-methyl-15-oxobicyclo[9.3.1]pentadecane-1-carboxylate
Fresu, Sonia; Schürmann, Markus; Preut, Hans; Eilbracht, Peter; Acta Crystallographica Section E 59 (2003) o1786–o1787; doi:10.1107/S1600536803023420

data_2202748
_publ_section_title
;Methyl
 <i>rac</i>-(1<i>S</i>*,11<i>R</i>*,12<i>S</i>*,14<i>S</i>*)-12-hydroxy-14-methyl-15-oxobicyclo[9.3.1]pentadecane-1-carboxylate
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1786
_journal_page_last               o1787
_journal_paper_doi               10.1107/S1600536803023420
_journal_volume                  59
_journal_year                    2003
_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
;
Methyl rac-(1S*,11R*,12S*,14S*)-12-hydroxy-14-methyl-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                89.9661(7)
_cell_angle_beta                 87.4671(8)
_cell_angle_gamma                75.2109(7)
_cell_formula_units_Z            2
_cell_length_a                   8.4865(5)
_cell_length_b                   8.8025(2)
_cell_length_c                   12.2034(2)
_cell_measurement_reflns_used    13476
_cell_measurement_temperature    291.0(10)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      3.37
_cell_volume                     880.51(6)
_computing_cell_refinement
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
DENZO and SCALEPACK
;
_computing_molecular_graphics    'SHELTXL-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 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
;
488 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  0.023
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13476
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         3.37
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             340
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.290
_refine_diff_density_min         -0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         4008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0417
_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^)+(0.0697P)^2^+0.0293P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1307
_reflns_number_gt                2991
_reflns_number_total             4008
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na6251.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               2202748
_cod_database_fobs_code          2202748