5-Amino-2,4,6-tribromoisophthalic acid: the MAD triangle for experimental phasing
Beck, Tobias; Herbst-Irmer, Regine; Sheldrick, George M.; Acta Crystallographica Section C 65 (2009) o237–o239; doi:10.1107/S0108270109013195

data_2017085
_publ_section_title
;
 5-Amino-2,4,6-tribromoisophthalic acid: the MAD triangle for
 experimental phasing
;
_journal_coeditor_code           EG3012
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o237
_journal_page_last               o239
_journal_paper_doi               10.1107/S0108270109013195
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          'C8 H4 Br3 N O4'
_chemical_formula_moiety         'C8 H4 Br3 N O4'
_chemical_formula_sum            'C8 H4 Br3 N O4'
_chemical_formula_weight         417.85
_chemical_name_systematic
;
5-Amino-2,4,6-tribromoisophthalic acid
;
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.69(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   16.728(2)
_cell_length_b                   11.449(2)
_cell_length_c                   23.649(3)
_cell_measurement_reflns_used    9995
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.361
_cell_measurement_theta_min      2.65
_cell_volume                     4464.6(12)
_computing_cell_refinement       'SAINT (Bruker 2007)'
_computing_data_collection       'APEX2 (Bruker 2007)'
_computing_data_reduction        'SAINT (Bruker 2007)'
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008) and PyMOL (DeLano, 2008)
;
_computing_publication_material
;
SHELXL97 (Sheldrick, 2008) and SHELXTL (Sheldrick, 2008)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.602
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker SMART 6000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  'INCOATEC multilayer optics'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_sigmaI/netI    0.0245
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            97602
_diffrn_reflns_theta_full        67.50
_diffrn_reflns_theta_max         73.98
_diffrn_reflns_theta_min         2.68
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    13.443
_exptl_absorpt_correction_T_max  0.5529
_exptl_absorpt_correction_T_min  0.3466
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(TWINABS; Sheldrick 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.487
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3136
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.546
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     626
_refine_ls_number_reflns         8717
_refine_ls_number_restraints     106
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0207P)^2^+12.7819P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0631
_refine_ls_wR_factor_ref         0.0641
_reflns_number_gt                8413
_reflns_number_total             8717
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            eg3012.cif
_cod_data_source_block           B3C
_cod_original_cell_volume        4464.6(11)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2017085