#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:14:58 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179445 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/42/4334282.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_4334282
loop_
_publ_author_name
'Alexander Yu. Makarov'
'Frank Blockhuys'
'Irina Yu. Bagryanskaya'
'Yuri V. Gatilov'
'Makhmut M. Shakirov'
'Andrey V. Zibarev'
_publ_contact_author_email       bagryan@nioch.nsc.ru
_publ_contact_author_name        'Dr. I. Yu. Bagryanskaya'
_publ_section_title
;
 Experimental and Computational Study on the Structure and Properties of
 Herz Cations and Radicals: 1,2,3-Benzodithiazolium,
 1,2,3-Benzodithiazolyl, and Their Se Congeners
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3699
_journal_page_last               3710
_journal_paper_doi               10.1021/ic302203t
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C6 H4 N Se2 1+, Cl4 Ga 1-'
_chemical_formula_sum            'C6 H4 Cl4 Ga N Se2'
_chemical_formula_weight         459.54
_chemical_melting_point          398
_chemical_name_systematic
; 
 1,2,3-benzodiselenazolium tetrachlorogallate 
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.8950(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4699(3)
_cell_length_b                   10.1981(3)
_cell_length_c                   17.0300(6)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      31.86
_cell_measurement_theta_min      2.91
_cell_volume                     1294.33(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            25594
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         32.35
_diffrn_reflns_theta_min         2.33
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.537
_exptl_absorpt_correction_T_max  0.9703
_exptl_absorpt_correction_T_min  0.6487
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.358
_exptl_crystal_description       prism
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.958
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         4280
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0228
_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/[σ²(Fo²)+(0.0220P)²+0.8323P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0496
_refine_ls_wR_factor_ref         0.0532
_reflns_number_gt                3648
_reflns_number_total             4280
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302203t_si_001_1.cif
_cod_data_source_block           m521
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4334282
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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 0.92100(3) 0.28944(2) 0.177499(13) 0.03352(5) Uani 1 1 d .
Ga1 Ga 1.44583(3) 0.191642(19) 0.382448(12) 0.02612(5) Uani 1 1 d .
Se2 Se 1.01666(3) 0.08436(2) 0.215717(13) 0.03370(6) Uani 1 1 d .
Cl1 Cl 1.45765(8) 0.33973(5) 0.47314(3) 0.03820(11) Uani 1 1 d .
Cl2 Cl 1.33868(8) 0.28114(5) 0.27132(3) 0.04009(12) Uani 1 1 d .
Cl3 Cl 1.71344(8) 0.11851(6) 0.36646(4) 0.04516(13) Uani 1 1 d .
Cl4 Cl 1.26753(9) 0.03349(6) 0.40904(4) 0.05251(16) Uani 1 1 d .
N1 N 0.8219(2) 0.00339(17) 0.18083(10) 0.0338(4) Uani 1 1 d .
C1 C 0.7092(3) 0.21532(19) 0.13591(11) 0.0280(4) Uani 1 1 d .
C2 C 0.6919(3) 0.07634(18) 0.14600(11) 0.0281(4) Uani 1 1 d .
C3 C 0.5294(3) 0.0145(2) 0.11558(13) 0.0366(4) Uani 1 1 d .
H3 H 0.5125 -0.0769 0.1227 0.044 Uiso 1 1 calc R
C4 C 0.4001(3) 0.0871(2) 0.07671(13) 0.0391(5) Uani 1 1 d .
H4 H 0.2924 0.0461 0.0567 0.047 Uiso 1 1 calc R
C5 C 0.4234(3) 0.2233(2) 0.06560(14) 0.0395(5) Uani 1 1 d .
H5 H 0.3316 0.2716 0.0371 0.047 Uiso 1 1 calc R
C6 C 0.5744(3) 0.2873(2) 0.09473(14) 0.0363(4) Uani 1 1 d .
H6 H 0.5873 0.3790 0.0871 0.044 Uiso 1 1 calc 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 0.02940(10) 0.02893(10) 0.04136(12) -0.00066(8) -0.00394(8) -0.00442(7)
Ga1 0.02849(10) 0.02293(9) 0.02669(10) -0.00198(7) 0.00005(8) -0.00146(7)
Se2 0.02882(10) 0.03102(10) 0.04026(11) -0.00357(8) -0.00495(8) 0.00142(7)
Cl1 0.0467(3) 0.0347(2) 0.0329(2) -0.01020(19) 0.0000(2) 0.0029(2)
Cl2 0.0429(3) 0.0407(3) 0.0345(2) 0.0064(2) -0.0130(2) -0.0125(2)
Cl3 0.0382(3) 0.0473(3) 0.0508(3) -0.0026(2) 0.0085(2) 0.0126(2)
Cl4 0.0561(4) 0.0394(3) 0.0623(4) 0.0077(3) 0.0057(3) -0.0195(3)
N1 0.0329(9) 0.0283(8) 0.0394(9) -0.0039(7) -0.0031(7) -0.0003(7)
C1 0.0279(9) 0.0284(9) 0.0280(9) -0.0026(7) 0.0035(7) -0.0008(7)
C2 0.0291(9) 0.0280(9) 0.0273(9) -0.0033(7) 0.0019(7) -0.0009(7)
C3 0.0343(10) 0.0340(10) 0.0409(11) -0.0054(8) -0.0015(9) -0.0057(8)
C4 0.0289(10) 0.0464(12) 0.0412(12) -0.0102(9) -0.0042(9) -0.0056(9)
C5 0.0325(10) 0.0450(12) 0.0400(12) -0.0028(9) -0.0059(9) 0.0049(9)
C6 0.0352(10) 0.0317(10) 0.0413(11) 0.0017(8) -0.0024(9) 0.0022(8)
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C1 Se1 Se2 88.73(6)
Cl1 Ga1 Cl4 111.62(3)
Cl1 Ga1 Cl3 109.72(2)
Cl4 Ga1 Cl3 110.89(3)
Cl1 Ga1 Cl2 108.66(2)
Cl4 Ga1 Cl2 107.24(3)
Cl3 Ga1 Cl2 108.61(2)
N1 Se2 Se1 95.67(6)
C2 N1 Se2 117.03(14)
C6 C1 C2 120.77(18)
C6 C1 Se1 123.13(15)
C2 C1 Se1 116.07(15)
N1 C2 C3 119.34(18)
N1 C2 C1 122.46(18)
C3 C2 C1 118.18(18)
C4 C3 C2 119.7(2)
C4 C3 H3 120.2
C2 C3 H3 120.2
C3 C4 C5 120.8(2)
C3 C4 H4 119.6
C5 C4 H4 119.6
C6 C5 C4 121.8(2)
C6 C5 H5 119.1
C4 C5 H5 119.1
C5 C6 C1 118.7(2)
C5 C6 H6 120.6
C1 C6 H6 120.6
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Se1 C1 1.850(2)
Se1 Se2 2.2902(3)
Ga1 Cl1 2.1577(5)
Ga1 Cl4 2.1593(6)
Ga1 Cl3 2.1680(6)
Ga1 Cl2 2.2022(6)
Se2 N1 1.7416(17)
N1 C2 1.330(3)
C1 C6 1.396(3)
C1 C2 1.435(3)
C2 C3 1.433(3)
C3 C4 1.354(3)
C3 H3 0.9500
C4 C5 1.414(3)
C4 H4 0.9500
C5 C6 1.367(3)
C5 H5 0.9500
C6 H6 0.9500
