#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:00:37 +0100 (lun 21 de mar de 2016) $
#$Revision: 178832 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/86/4108603.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4108603
loop_
_publ_author_name
'Craig M. Robertson'
'Alicea A. Leitch'
'Kristina Cvrkalj'
'Daniel J. T. Myles'
'Robert W. Reed'
'Paul A. Dube'
'Richard T. Oakley'
_publ_section_title
;
 Ferromagnetic Ordering in Bisthiaselenazolyl Radicals: Variations on a
 Tetragonal Theme
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14791
_journal_page_last               14801
_journal_paper_doi               10.1021/ja8054436
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C7 H5 Br N3 S2 Se2'
_chemical_formula_weight         433.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           113
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P -4 2ab'
_symmetry_space_group_name_H-M   'P -4 21 m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0499(7)
_cell_length_b                   16.0499(7)
_cell_length_c                   4.0684(3)
_cell_measurement_reflns_used    3885
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.04
_cell_measurement_theta_min      2.84
_cell_volume                     1048.02(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD Camera'
_diffrn_measurement_method       'omega scans'
_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  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0421
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -3
_diffrn_reflns_number            5463
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         2.84
_exptl_absorpt_coefficient_mu    11.231
_exptl_absorpt_correction_T_max  0.6422
_exptl_absorpt_correction_T_min  0.1069
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'APEX II'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.745
_exptl_crystal_description       Needle
_exptl_crystal_F_000             812
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.888
_refine_diff_density_min         -0.866
_refine_diff_density_rms         0.135
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.061(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         1196
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0333P)²+0.3858P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0662
_reflns_number_gt                1151
_reflns_number_total             1196
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8054436_si_008.cif
_cod_data_source_block           brbptset-lt_0m
_cod_database_code               4108603
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'-y+1/2, -x+1/2, z'
'y+1/2, x+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Se1 Se 0.43954(3) 0.60200(2) 0.76552(12) 0.00945(13) Uani 1 1 d .
S1 S 0.46956(7) 0.72695(7) 0.5448(3) 0.0095(2) Uani 1 1 d .
N1 N 0.3393(2) 0.6354(3) 0.9300(11) 0.0108(9) Uani 1 1 d .
C1 C 0.3197(3) 0.7124(3) 0.8521(12) 0.0074(9) Uani 1 1 d U
C2 C 0.3728(3) 0.7661(3) 0.6640(11) 0.0079(9) Uani 1 1 d .
Br1 Br 0.41847(3) 0.91847(3) 0.35418(16) 0.01269(17) Uani 1 2 d S
N2 N 0.2438(2) 0.7438(2) 0.9577(13) 0.0074(11) Uani 1 2 d S
C3 C 0.3466(3) 0.8466(3) 0.5824(17) 0.0107(13) Uani 1 2 d S
C4 C 0.1910(3) 0.6910(3) 1.1729(16) 0.0075(10) Uani 1 2 d SU
H4A H 0.2265 0.6583 1.3119 0.009 Uiso 1 1 d R
C5 C 0.1334(3) 0.6334(3) 0.9850(18) 0.0139(14) Uani 1 2 d S
H5A H 0.1012 0.6012 1.1379 0.021 Uiso 1 2 d SR
H5B H 0.1658 0.5962 0.8493 0.021 Uiso 1 1 d R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Se1 0.0091(2) 0.0094(2) 0.0098(2) -0.00039(18) 0.00006(18) 0.00095(16)
S1 0.0080(5) 0.0082(5) 0.0124(6) 0.0009(4) 0.0020(4) 0.0018(4)
N1 0.0071(18) 0.0121(19) 0.013(2) 0.0003(16) -0.0036(16) -0.0001(16)
C1 0.0077(12) 0.0078(12) 0.0066(12) -0.0003(9) -0.0002(9) -0.0006(9)
C2 0.0083(19) 0.012(2) 0.004(2) -0.0011(17) -0.0004(17) -0.0015(18)
Br1 0.0111(2) 0.0111(2) 0.0159(4) 0.00318(17) 0.00318(17) -0.0011(3)
N2 0.0083(15) 0.0083(15) 0.006(3) 0.0006(14) 0.0006(14) -0.004(2)
C3 0.014(2) 0.014(2) 0.005(3) 0.0013(18) 0.0013(18) -0.008(3)
C4 0.0077(10) 0.0077(10) 0.0069(14) 0.0003(7) 0.0003(7) -0.0004(9)
C5 0.014(2) 0.014(2) 0.013(4) 0.0046(19) 0.0046(19) -0.003(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Se1 S1 94.20(13) . .
C2 S1 Se1 91.09(15) . .
C1 N1 Se1 113.5(3) . .
N1 C1 N2 118.5(4) . .
N1 C1 C2 123.5(4) . .
N2 C1 C2 118.0(4) . .
C3 C2 C1 120.2(4) . .
C3 C2 S1 122.3(4) . .
C1 C2 S1 117.5(3) . .
C1 N2 C1 122.8(6) . 8_455
C1 N2 C4 118.5(3) . .
C1 N2 C4 118.5(3) 8_455 .
C2 C3 C2 119.9(6) . 8_455
C2 C3 Br1 120.0(3) . .
C2 C3 Br1 120.0(3) 8_455 .
N2 C4 C5 113.5(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Se1 N1 1.823(4) .
Se1 S1 2.2494(12) .
S1 C2 1.744(4) .
N1 C1 1.314(6) .
C1 N2 1.387(5) .
C1 C2 1.432(6) .
C2 C3 1.399(5) .
Br1 C3 1.877(7) .
N2 C1 1.387(5) 8_455
N2 C4 1.484(8) .
C3 C2 1.399(5) 8_455
C4 C5 1.515(9) .
