7,7-Dimethyl-3,3,4a-tris(3-methylbut-2-enyl)-4a,5,6,7-tetrahydro-2<i>H</i>-chromene-2,4(3<i>H</i>)-dione
Möws, Katrin; Schürmann, Markus; Preut, Hans; Plietker, Bernd; Acta Crystallographica Section E 65 (2009) o1751–; doi:10.1107/S1600536809025021

data_2222701
_publ_section_title
7,7-Dimethyl-3,3,4a-tris(3-methylbut-2-enyl)-4a,5,6,7-tetrahydro-2<i>H</i>-chromene-2,4(3<i>H</i>)-dione
_journal_coeditor_code           HB5012
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1751
_journal_paper_doi               10.1107/S1600536809025021
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C26 H38 O3'
_chemical_formula_moiety         'C26 H38 O3'
_chemical_formula_sum            'C26 H38 O3'
_chemical_formula_weight         398.56
_chemical_name_systematic
;
7,7-Dimethyl-3,3,4a-tris(3-methylbut-2-enyl)-4a,5,6,7-tetrahydro-2<i>H</i>-
chromene-2,4(3<i>H</i>)-dione
;
_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                77.862(13)
_cell_angle_beta                 78.325(12)
_cell_angle_gamma                66.427(9)
_cell_formula_units_Z            2
_cell_length_a                   9.534(2)
_cell_length_b                   11.753(3)
_cell_length_c                   11.994(2)
_cell_measurement_reflns_used    14072
_cell_measurement_temperature    173.0(10)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      3.11
_cell_volume                     1193.7(5)
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method
;
415 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  0.078
_diffrn_reflns_av_sigmaI/netI    0.3033
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14072
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.11
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.109
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.106
_refine_diff_density_min         -0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4134
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1665
_refine_ls_R_factor_gt           0.0363
_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= {exp[6.80(sin\q/\l)^2^]}/[\s^2^(Fo^2^)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.1117
_reflns_number_gt                1323
_reflns_number_total             4134
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hb5012.cif
_cod_data_source_block           I
_cod_database_code               2222701
_cod_database_fobs_code          2222701