Structural phase transitions, and Br···N and Br···Br interactions in 1-phenyl-2-methyl-4-nitro-5-bromoimidazole
Kubicki, Maciej; Acta Crystallographica Section B 60 (2004) 333–342; doi:10.1107/S0108768104005853

data_2102505
_publ_section_title
;
 Structural phase transitions, and Br&#x00B7;&#x00B7;&#x00B7;N and
 Br&#x00B7;&#x00B7;&#x00B7;Br interactions in
 1-phenyl-2-methyl-4-nitro-5-bromoimidazole
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              333
_journal_page_last               342
_journal_paper_doi               10.1107/S0108768104005853
_journal_volume                  60
_journal_year                    2004
_chemical_formula_moiety         'C10 H8 Br N3 O2'
_chemical_formula_sum            'C10 H8 Br N3 O2'
_chemical_formula_weight         282.10
_chemical_name_systematic
;
1-phenyl-4-nitro-5-bromo-imidazole
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.478(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.9723(5)
_cell_length_b                   6.8169(4)
_cell_length_c                   22.9000(12)
_cell_measurement_reflns_used    3121
_cell_measurement_temperature    120.0(10)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      3
_cell_volume                     1043.72(12)
_computing_cell_refinement       'CrysAlisCCD v.169 (Oxford Diffraction, 2003a)'
_computing_data_collection       'CrysAlisCCD v.169 (Oxford Diffraction, 2003a)'
_computing_data_reduction        'CrysAlisRed v.169 (Oxford Diffraction, 2003b)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120.0(10)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measurement_device_type  'KUMA KM4CCD four-circle diffractometer'
_diffrn_measurement_method       \w-scan
_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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0303
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            13861
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.81
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    3.926
_exptl_absorpt_correction_T_max  0.573
_exptl_absorpt_correction_T_min  0.378
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SORTAV (Blessing, 1989)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.711
_refine_diff_density_min         -0.517
_refine_ls_extinction_coef       0.0095(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         2788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0329
_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^)+(0.0000P)^2^+2.8500P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0651
_refine_ls_wR_factor_ref         0.0678
_reflns_number_gt                2349
_reflns_number_total             2788
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            bk5005.cif
_cod_data_source_block           120K
_cod_original_cell_volume        1043.72(11)
_cod_original_sg_symbol_H-M      P2~1~/c
_cod_database_code               2102505