Crystal Structure of 3,8-Dibromo-3-(bromomethyl)-3,3a,4,5,6,6a-hexahydro-6a-hydroxy-6,9a-dimethylazuleno[4,5-b]furan-2,9-dione—A Sesquiterpene Lactone
KAPOOR, Kamini; GUPTA, Vivek K.; SHAH, Bhahwal A.; ANDOTRA, Samar S.; TANEJA, Subhash C.; X-ray Structure Analysis Online 27 (2011) 67–; doi:10.2116/xraystruct.27.67

data_1551738
_publ_section_title
;
 Crystal Structure of
 3,8-Dibromo-3-(bromomethyl)-3,3a,4,5,6,6a-hexahydro-6a-hydroxy-6,9a-dimethylazuleno[4,5-b]furan-2,9-dione---A
 Sesquiterpene Lactone
;
_journal_name_full               'X-ray Structure Analysis Online'
_journal_page_first              67
_journal_paper_doi               10.2116/xraystruct.27.67
_journal_volume                  27
_journal_year                    2011
_chemical_formula_moiety         'C15 H17 Br3 O4'
_chemical_formula_sum            'C15 H17 Br3 O4'
_chemical_formula_weight         501.02
_chemical_name_systematic
;
 5,10-dimethyl-1-hydroxy-3,11,13-tribromo
-hexahydroazulino[6,7-b] furan-4,12-dione
;
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_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                 109.246(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.9170(6)
_cell_length_b                   10.7305(6)
_cell_length_c                   10.4145(8)
_cell_measurement_reflns_used    3802
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.8683
_cell_measurement_theta_min      3.7901
_cell_volume                     835.30(11)
_computing_cell_refinement       'CrysAlisPro,Oxford Diff.Ltd,Ver 1.171.34.40'
_computing_data_collection       'CrysAlisPro,Oxford Diff.Ltd,Ver 1.171.34.40'
_computing_data_reduction        'CrysAlisPro,Oxford Diff.Ltd,Ver 1.171.34.40'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'PLATON(Spek,1999)& PARST(1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.1049
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'omega scans'
_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  0.0450
_diffrn_reflns_av_sigmaI/netI    0.0660
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6651
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.93
_exptl_absorpt_coefficient_mu    7.258
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Crys Alis Red'
_exptl_crystal_colour            'light brown'
_exptl_crystal_density_diffrn    1.992
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.030(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2839
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0623P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1131
_reflns_number_gt                2342
_reflns_number_total             2839
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            27_67_1.cif
_cod_data_source_block           bhaw5
_cod_original_cell_volume        835.30(10)
_cod_original_sg_symbol_H-M      P21
_cod_database_code               1551738