Ethyl hydrogen 4,5-dibromophthalate
Britton, Doyle; Acta Crystallographica Section C 55 (1999) IUC9900071–; doi:10.1107/S0108270199099229

data_2008710
_publ_section_title
;
 Ethyl hydrogen 4,5-dibromophthalate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              IUC9900071
_journal_paper_doi               10.1107/S0108270199099229
_journal_volume                  55
_journal_year                    1999
_chemical_formula_sum            'C10 H8 Br2 O4'
_chemical_formula_weight         351.98
_chemical_melting_point          414.0(10)
_chemical_name_systematic
;
 4,5-dibromophthalic acid monoethylester
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_audit_creation_method           'SHELXL + manual additions'
_cell_angle_alpha                90.00
_cell_angle_beta                 101.69
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   5.1387(2)
_cell_length_b                   22.5026(10)
_cell_length_c                   10.1410(4)
_cell_measurement_reflns_used    3870
_cell_measurement_temperature    174(2)
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      1.8
_cell_volume                     1148.32(8)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'ASTRO (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1994)'
_diffrn_ambient_temperature      174(2)
_diffrn_measurement_device       'Siemens SMART area-detector'
_diffrn_measurement_method       \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  0.034
_diffrn_reflns_av_sigmaI/netI    0.0398
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5644
_diffrn_reflns_theta_max         24.93
_diffrn_reflns_theta_min         1.81
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_time
;
 The first 130 reflections were remeasured at the end of
 the data collection 10 h later.
;
_diffrn_standards_number         130
_exptl_absorpt_coefficient_mu    7.054
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.55
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996; Blessing, 1995)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.036
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
;
The crystals grew as flat needles elongated along a with faces (011).
;
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.662
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.095
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment
'H atoms riding with U = 1.2U(average) of the attached atom'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1988
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_restrained_S_obs      1.132
_refine_ls_R_factor_all          0.046
_refine_ls_R_factor_gt           0.035
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          -0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.034P)^2^+1.15P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.078
_refine_ls_wR_factor_ref         0.074
_reflns_number_gt                1703
_reflns_number_total             1988
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            qa0129.cif
_cod_data_source_block           IUC9900071
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '413-415 K' was changed to
'414.0(10)' - the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '413-415 K' was changed to
'414.0(10)' - the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.034P)^2^+1.15P] where P = (Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.034P)^2^+1.15P] where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1148.34(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2008710