5-Chloro- and 5-bromobenzfurazan 1-oxide revisited
Pink, Maren; Britton, Doyle; Acta Crystallographica Section B 58 (2002) 116–124; doi:10.1107/S0108768101014744

data_2103146
_publ_section_title
;
 5-Chloro- and 5-bromobenzfurazan 1-oxide revisited
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              116
_journal_page_last               124
_journal_paper_doi               10.1107/S0108768101014744
_journal_volume                  58
_journal_year                    2002
_chemical_formula_sum            'C6 H3 Br N2 O2'
_chemical_formula_weight         215.01
_chemical_name_systematic
;
 5-bromobenzfurazan-1-oxide  (high temperature polymorph)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXTL  plus manual additions'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.124(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.954(4)
_cell_length_b                   7.297(3)
_cell_length_c                   12.574(6)
_cell_measurement_reflns_used    1671
_cell_measurement_temperature    299.0(10)
_cell_measurement_theta_max      21.7
_cell_measurement_theta_min      2.8
_cell_volume                     729.8(6)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXLTL
_computing_publication_material  SHELXLTL
_computing_structure_refinement  SHELXLTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1994)'
_diffrn_ambient_temperature      299.0(10)
_diffrn_measurement_device
;
Siemens SMART area-detector diffractometer
;
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .0299
_diffrn_reflns_av_sigmaI/netI    .0322
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5494
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         3.03
_diffrn_standards_decay_%        2.1
_diffrn_standards_interval_time  '6 hours'
_diffrn_standards_number         69
_exptl_absorpt_coefficient_mu    5.576
_exptl_absorpt_correction_T_max  .57
_exptl_absorpt_correction_T_min  .30
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS; Sheldrick, 1996; Blessing, 1995
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.957
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             416
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .10
_refine_diff_density_max         .567
_refine_diff_density_min         -.535
_refine_ls_extinction_coef       .013(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXTL
_refine_ls_goodness_of_fit_all   .950
_refine_ls_goodness_of_fit_obs   1.221
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         1650
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      .943
_refine_ls_restrained_S_obs      1.199
_refine_ls_R_factor_all          .0821
_refine_ls_R_factor_obs          .0464
_refine_ls_shift/esd_max         .001
_refine_ls_shift/esd_mean        .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.084P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .1391
_refine_ls_wR_factor_obs         .1271
_reflns_number_observed          896
_reflns_number_total             1650
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            bk0096.cif
_cod_data_source_block           Br299K
_cod_original_cell_volume        729.9(6)
_cod_original_sg_symbol_H-M      P2~1~/n
_cod_database_code               2103146
_cod_database_fobs_code          2103146