5-[(2-Bromophenylamino)methylene]-2,2-dimethyl-1,3-dioxane-4,6-dione
Silva, Luiz Everson da; Joussef, Antonio Carlos; Nunes, Ricardo José; Andrighetti-Fröhner, Carla Regina; Bortoluzzi, Adailton José; Acta Crystallographica Section E 61 (2005) o4252–o4253; doi:10.1107/S1600536805036883

data_2207453
_publ_section_title
;
 5-[(2-Bromophenylamino)methylene]-2,2-dimethyl-1,3-dioxane-4,6-dione
;
_journal_coeditor_code           BT6779
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4252
_journal_page_last               o4253
_journal_paper_doi               10.1107/S1600536805036883
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C13 H12 Br N O4'
_chemical_formula_moiety         'C13 H12 Br N O4'
_chemical_formula_sum            'C13 H12 Br N O4'
_chemical_formula_weight         326.15
_chemical_name_systematic
;
5-[(2-Bromophenylamino)methylene]-2,2-dimethyl-1,3-dioxane-4,6-dione
;
_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                95.570(5)
_cell_angle_beta                 101.043(5)
_cell_angle_gamma                99.508(5)
_cell_formula_units_Z            2
_cell_length_a                   6.960(5)
_cell_length_b                   9.298(5)
_cell_length_c                   10.424(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      16.91
_cell_measurement_theta_min      4.09
_cell_volume                     647.2(7)
_computing_cell_refinement
;
CAD-4/PC Software
;
_computing_data_collection
;
CAD-4/PC Software (Enraf--Nonius, 1993)
;
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_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      193(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \w--2\q
_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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0432
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2451
_diffrn_reflns_theta_full        25.07
_diffrn_reflns_theta_max         25.07
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.185
_exptl_absorpt_correction_T_max  0.601
_exptl_absorpt_correction_T_min  0.417
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>,  1968)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.674
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             328
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.386
_refine_ls_extinction_coef       0.024(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     177
_refine_ls_number_reflns         2312
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0651
_refine_ls_R_factor_gt           0.0302
_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^)+(0.0298P)^2^+0.241P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                1724
_reflns_number_total             2312
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6779.cif
_cod_data_source_block           I
_cod_database_code               2207453
_cod_database_fobs_code          2207453