<i>rac</i>-(<i>Z</i>)-Ethyl 2-bromo-2-[(3<i>R</i>,5<i>R</i>)-3-bromo-5-methyltetrahydrofuran-2-ylidene]acetate
François Loiseau; Reinhard Neier; Gaël Labat; Helen Stoeckli-Evans; Acta Crystallographica Section C 62 (2006) o636–o638; doi:10.1107/S0108270106037127

data_2015640
_publ_section_title
;<i>rac</i>-(<i>Z</i>)-Ethyl
 2-bromo-2-[(3<i>R</i>,5<i>R</i>)-3-bromo-5-methyltetrahydrofuran-2-ylidene]acetate
;
_journal_coeditor_code           GA3026
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o636
_journal_page_last               o638
_journal_paper_doi               10.1107/S0108270106037127
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C9 H12 Br2 O3'
_chemical_formula_moiety         'C9 H12 Br2 O3'
_chemical_formula_sum            'C9 H12 Br2 O3'
_chemical_formula_weight         328.01
_chemical_name_systematic
;
rac-(Z)-Ethyl
2-bromo-2-[(3R,5R)-3-bromo-5-methyltetrahydrofuran-2-ylidene]acetate
;
_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                85.740(7)
_cell_angle_beta                 82.209(7)
_cell_angle_gamma                64.386(7)
_cell_formula_units_Z            4
_cell_length_a                   9.0779(8)
_cell_length_b                   9.1402(9)
_cell_length_c                   15.3942(13)
_cell_measurement_reflns_used    12061
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.55
_cell_measurement_theta_min      2.47
_cell_volume                     1140.98(19)
_computing_cell_refinement       X-AREA
_computing_data_collection       'X-AREA (Stoe & Cie, 2005)'
_computing_data_reduction        'X-RED32 (Stoe & Cie, 2005)'
_computing_molecular_graphics    'PLATON  (Spek, 2003)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Stoe IPDS-2'
_diffrn_measurement_method       '\f and \w'
_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  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0617
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17073
_diffrn_reflns_theta_full        29.21
_diffrn_reflns_theta_max         29.21
_diffrn_reflns_theta_min         2.47
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.085
_exptl_absorpt_correction_T_max  0.245
_exptl_absorpt_correction_T_min  0.126
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS in PLATON; Spek, 2003)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.909
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.828
_refine_diff_density_min         -1.192
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.900
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         6151
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.900
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0400
_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^)+(0.0485P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0808
_refine_ls_wR_factor_ref         0.0881
_reflns_number_gt                4464
_reflns_number_total             6151
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ga3026.cif
_cod_data_source_block           IV
_cod_original_cell_volume        1140.98(18)
_cod_database_code               2015640
_cod_database_fobs_code          2015640