(3<i>R</i>,4<i>S</i>,5<i>S</i>)-4-Hydroxy-3-methyl-5-[(2<i>S</i>,3<i>R</i>)-3-methylpent-4-en-2-yl]tetrahydrofuran-2-one
Becker, Annika; Schürmann, Markus; Preut, Hans; Hiersemann, Martin; Acta Crystallographica Section E 64 (2008) o1517–; doi:10.1107/S1600536808021181

data_2219009
_publ_section_title
(3<i>R</i>,4<i>S</i>,5<i>S</i>)-4-Hydroxy-3-methyl-5-[(2<i>S</i>,3<i>R</i>)-3-methylpent-4-en-2-yl]tetrahydrofuran-2-one
_journal_coeditor_code           HB2741
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1517
_journal_paper_doi               10.1107/S1600536808021181
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C11 H18 O3'
_chemical_formula_moiety         'C11 H18 O3'
_chemical_formula_sum            'C11 H18 O3'
_chemical_formula_weight         198.25
_chemical_name_systematic
;
(3<i>R</i>,4<i>S</i>,5<i>S</i>)-4-Hydroxy-3-methyl-5-[(2<i>S</i>,3<i>R</i>)-
3-methylpent-4-en-2-yl]tetrahydrofuran-2-one
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 95.46(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.2934(13)
_cell_length_b                   16.411(3)
_cell_length_c                   11.607(2)
_cell_measurement_reflns_used    9263
_cell_measurement_temperature    291.0(10)
_cell_measurement_theta_max      25.38
_cell_measurement_theta_min      3.04
_cell_volume                     1193.3(4)
_computing_cell_refinement
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection       'COLLECT (Nonius, 1998)'
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and PLATON (Spek, 2003)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      291.0(10)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
;
259  frames via \w-rotation (\D\w=1%) and two times 120 s per frame
(three 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  0.026
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9263
_diffrn_reflns_theta_full        25.38
_diffrn_reflns_theta_max         25.38
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.103
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             432
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.136
_refine_diff_density_min         -0.099
_refine_ls_extinction_coef       0.042(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         2268
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0823
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0276P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0796
_reflns_number_gt                1228
_reflns_number_total             2268
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb2741.cif
_cod_data_source_block           I
_cod_original_cell_volume        1193.4(4)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2219009
_cod_database_fobs_code          2219009