(3<i>S</i>*,4<i>S</i>*,<i>E</i>)-<i>tert</i>-Butyl 3,4-dibromo-5-oxocyclooct-1-enecarboxylate
Blanco, Magda; Garrido, Narciso M.; Sanz, Francisca; Diez, David; Acta Crystallographica Section E 68 (2012) o232–; doi:10.1107/S1600536811053852

data_2233106
_publ_section_title
;
 (3<i>S</i>*,4<i>S</i>*,<i>E</i>)-<i>tert</i>-Butyl
 3,4-dibromo-5-oxocyclooct-1-enecarboxylate
;
_journal_coeditor_code           BT5753
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o232
_journal_paper_doi               10.1107/S1600536811053852
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          'C13 H18 Br2 O3'
_chemical_formula_moiety         'C13 H18 Br2 O3'
_chemical_formula_sum            'C13 H18 Br2 O3'
_chemical_formula_weight         382.09
_chemical_name_systematic
;
(3<i>S</i>*,4<i>S</i>*,<i>E</i>)-<i>tert</i>-Butyl
3,4-dibromo-5-oxocyclooct-1-enecarboxylate
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.0658(4)
_cell_length_b                   9.5990(3)
_cell_length_c                   11.2657(3)
_cell_measurement_reflns_used    9578
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      66.47
_cell_measurement_theta_min      4.61
_cell_volume                     1521.07(8)
_computing_cell_refinement       'SAINT (Bruker 2006)'
_computing_data_collection       'APEX2 (Bruker 2006)'
_computing_data_reduction        'SAINT (Bruker 2006)'
_computing_molecular_graphics    'Mercury (Macrae <i>et al.</i>, 2006)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_av_sigmaI/netI    0.0473
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            10215
_diffrn_reflns_theta_full        66.47
_diffrn_reflns_theta_max         66.47
_diffrn_reflns_theta_min         4.61
_exptl_absorpt_coefficient_mu    6.756
_exptl_absorpt_correction_T_max  0.509
_exptl_absorpt_correction_T_min  0.370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2006)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.461
_refine_ls_abs_structure_details 'Flack (1983), 803 Friedel pairs'
_refine_ls_abs_structure_Flack   0.06(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2170
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0448P)^2^+0.2923P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0746
_reflns_number_gt                2153
_reflns_number_total             2170
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt5753.cif
_cod_data_source_block           I
_cod_database_code               2233106
_cod_database_fobs_code          2233106