7,7-Dimethyl-4a-(3-methyl-2-butenyl)-2-oxo-4a,5,6,7-tetrahydro-2<i>H</i>-chromen-4-yl benzoate
Möws, Katrin; Schürmann, Markus; Preut, Hans; Plietker, Bernd; Acta Crystallographica Section E 65 (2009) o2139–; doi:10.1107/S1600536809030918

data_2223093
_publ_section_title
;7,7-Dimethyl-4a-(3-methyl-2-butenyl)-2-oxo-4a,5,6,7-tetrahydro-2<i>H</i>-chromen-4-yl
 benzoate
;
_journal_coeditor_code           HG2544
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o2139
_journal_paper_doi               10.1107/S1600536809030918
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C23 H26 O4'
_chemical_formula_moiety         'C23 H26 O4'
_chemical_formula_sum            'C23 H26 O4'
_chemical_formula_weight         366.44
_chemical_name_systematic
;
7,7-Dimethyl-4a-(3-methyl-2-butenyl)-2-oxo-4a,5,6,7-tetrahydro-2<i>H</i>-
chromen-4-yl benzoate
;
_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                69.23(2)
_cell_angle_beta                 83.649(17)
_cell_angle_gamma                74.823(17)
_cell_formula_units_Z            2
_cell_length_a                   9.559(4)
_cell_length_b                   10.201(5)
_cell_length_c                   11.087(5)
_cell_measurement_reflns_used    12656
_cell_measurement_temperature    173.0(10)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.93
_cell_volume                     975.4(8)
_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, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.0(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
;
239 frames via \w-rotation (\D\w=2\%) 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  0.065
_diffrn_reflns_av_sigmaI/netI    0.1279
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            12665
_diffrn_reflns_theta_full        25.30
_diffrn_reflns_theta_max         25.30
_diffrn_reflns_theta_min         2.93
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.174
_refine_diff_density_min         -0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.805
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.805
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0426
_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^)]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0618
_refine_ls_wR_factor_ref         0.0668
_reflns_number_gt                1691
_reflns_number_total             3547
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            hg2544.cif
_cod_data_source_block           I
_cod_database_code               2223093
_cod_database_fobs_code          2223093