Crystal structure of methyl 2-(2<i>H</i>-1,3-benzodioxol-5-yl)-7,9-dibromo-8-oxo-1-oxaspiro[4.5]deca-2,6,9-triene-3-carboxylate
Martins, Lucimara Julio; de Simoni, Deborah; Aparicio, Ricardo; Coelho, Fernando; Acta Crystallographica Section E 70 (2014) o1275–o1276; doi:10.1107/S1600536814024763

data_2240249
_publ_section_title
;
 Crystal structure of methyl
 2-(2<i>H</i>-1,3-benzodioxol-5-yl)-7,9-dibromo-8-oxo-1-oxaspiro[4.5]deca-2,6,9-triene-3-carboxylate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o1275
_journal_page_last               o1276
_journal_paper_doi               10.1107/S1600536814024763
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C18 H12 Br2 O6'
_chemical_formula_moiety         'C18 H12 Br2 O6'
_chemical_formula_sum            'C18 H12 Br2 O6'
_chemical_formula_weight         484.10
_chemical_name_systematic
2-(2<i>H</i>-1,3-Benzodioxol-5-yl)-7,9-dibromo-8-oxo-1-oxaspiro[4.5]deca-2,6,9-triene-3-carboxylate
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                84.485(4)
_cell_angle_beta                 80.007(5)
_cell_angle_gamma                78.077(4)
_cell_formula_units_Z            2
_cell_length_a                   8.1929(13)
_cell_length_b                   8.4811(14)
_cell_length_c                   12.761(2)
_cell_measurement_reflns_used    9887
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.1
_cell_measurement_theta_min      3.2
_cell_volume                     852.7(2)
_computing_cell_refinement
;
<i>SAINT</i> (Bruker, 2010)
;
_computing_data_collection
;
<i>APEX2</i> (Bruker, 2010)
;
_computing_data_reduction
;
<i>SAINT</i> (Bruker, 2010)
;
_computing_molecular_graphics
;
Mercury (Macrae <i>et al.</i>,  2006)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2003), PLATON (Spek, 2009) and
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXLE (H\"ubschle et al, 2011) and SHELXL2014 (Sheldrick,
2008)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX CCD detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            27788
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.338
_diffrn_reflns_theta_min         3.031
_exptl_absorpt_coefficient_mu    4.787
_exptl_absorpt_correction_T_max  0.5147
_exptl_absorpt_correction_T_min  0.3087
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2010)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.885
_exptl_crystal_description       block
_exptl_crystal_F_000             476
_exptl_crystal_size_max          0.321
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.390
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         7098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0230
_refine_ls_R_factor_gt           0.0181
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+0.2583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0455
_refine_ls_wR_factor_ref         0.0472
_reflns_number_gt                6288
_reflns_number_total             7098
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hg5413sup1.cif
_cod_data_source_block           I
_cod_database_code               2240249
_cod_database_fobs_code          2240249
_shelx_estimated_absorpt_t_min   0.309
_shelx_estimated_absorpt_t_max   0.515
_shelx_hkl_checksum              51115
_shelx_res_checksum              53950
_shelxl_version_number           2.014