Ethyl 1,3-dibromoazulene-6-carboxylate
Hussain, Zakir; Oeser, Thomas; Hopf, Henning; Acta Crystallographica Section E 61 (2005) o478–o479; doi:10.1107/S1600536805001972

data_2205140
_publ_section_title
;
 Ethyl 1,3-dibromoazulene-6-carboxylate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o478
_journal_page_last               o479
_journal_paper_doi               10.1107/S1600536805001972
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C13 H10 Br2 O2'
_chemical_formula_moiety         'C13 H10 Br2 O2'
_chemical_formula_sum            'C13 H10 Br2 O2'
_chemical_formula_weight         358.03
_chemical_name_systematic
;
Ethyl 1,3-dibromoazulene-6-carboxylate
;
_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                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            8
_cell_length_a                   17.032(2)
_cell_length_b                   3.9694(5)
_cell_length_c                   35.819(5)
_cell_measurement_reflns_used    12806
_cell_measurement_temperature    95(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.46
_cell_volume                     2421.6(5)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2001)'
_diffrn_ambient_temperature      95(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker Smart APEX CCD area-detector'
_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  0.039
_diffrn_reflns_av_sigmaI/netI    0.046
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            15805
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    6.680
_exptl_absorpt_correction_T_max  0.6170
_exptl_absorpt_correction_T_min  0.2657
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(SMART; Bruker, 2001)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.964
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.013
_refine_diff_density_min         -1.591
_refine_ls_abs_structure_details 'Flack (1983), 2880 Friedel pairs'
_refine_ls_abs_structure_Flack   0.141(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     310
_refine_ls_number_reflns         5943
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.044
_refine_ls_R_factor_gt           0.042
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0295P)^2^+8.7967P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.091
_refine_ls_wR_factor_ref         0.092
_reflns_number_gt                5714
_reflns_number_total             5943
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ob6470.cif
_cod_data_source_block           I
_cod_database_code               2205140
_cod_database_fobs_code          2205140