#------------------------------------------------------------------------------
#$Date: 2016-02-21 01:03:34 +0100 (dom 21 de feb de 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/75/2237502.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2237502
loop_
_publ_author_name
'Sun, Zan'
'Hu, Dong-Cheng'
'Liu, Jia-Cheng'
_publ_section_title
;
 1,3-Dimethyl-1H-1,2,3-benzotriazol-3-ium tetrachloridoferrate(III)
;
_journal_coeditor_code           HY2615
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m148
_journal_paper_doi               10.1107/S1600536813003711
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '(C8 H10 N3) [Fe Cl4]'
_chemical_formula_moiety         'C8 H10 N3 +, Cl4 Fe -'
_chemical_formula_sum            'C8 H10 Cl4 Fe N3'
_chemical_formula_weight         345.84
_chemical_name_systematic
;
1,3-Dimethyl-1H-1,2,3-benzotriazol-3-ium tetrachloridoferrate(III)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   10.2920(5)
_cell_length_b                   12.5518(6)
_cell_length_c                   22.5857(9)
_cell_measurement_reflns_used    1751
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.54
_cell_measurement_theta_min      3.13
_cell_volume                     2917.7(2)
_computing_cell_refinement       'CrysAlis PRO (Oxford Diffraction, 2012)'
_computing_data_collection       'CrysAlis PRO (Oxford Diffraction, 2012)'
_computing_data_reduction        'CrysAlis PRO (Oxford Diffraction, 2012)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Oxford Diffraction SuperNova (Dual, Cu at zero, Eos)'
_diffrn_measurement_method       'ω 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  0.0311
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            8114
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         26.50
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    1.744
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Oxford Diffraction, 2012)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.575
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.392
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         3016
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0923
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0779P)²+1.0720P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1516
_refine_ls_wR_factor_ref         0.1825
_reflns_number_gt                1828
_reflns_number_total             3016
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hy2615.cif
_cod_data_source_block           I
_cod_database_code               2237502
_cod_database_fobs_code          2237502
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
N N1 0.2130(5) 0.5085(4) 0.3377(2) 0.0934(14) Uani d . 1 1
N N2 0.1550(5) 0.5572(4) 0.3863(2) 0.0907(14) Uani d . 1 1
N N3 0.2259(5) 0.5203(4) 0.4309(2) 0.0912(13) Uani d . 1 1
C C1 0.3237(4) 0.4541(4) 0.4130(2) 0.0650(11) Uani d . 1 1
C C2 0.4177(6) 0.3997(5) 0.4452(2) 0.0927(17) Uani d . 1 1
H H2 0.4238 0.4034 0.4863 0.111 Uiso calc R 1 1
C C3 0.5016(6) 0.3393(5) 0.4106(3) 0.0986(17) Uani d . 1 1
H H3 0.5669 0.3006 0.4293 0.118 Uiso calc R 1 1
C C4 0.4922(6) 0.3345(6) 0.3510(3) 0.1023(18) Uani d . 1 1
H H4 0.5522 0.2937 0.3302 0.123 Uiso calc R 1 1
C C5 0.3950(6) 0.3889(5) 0.3193(2) 0.0877(16) Uani d . 1 1
H H5 0.3874 0.3845 0.2783 0.105 Uiso calc R 1 1
C C6 0.3140(6) 0.4478(5) 0.3524(2) 0.0823(15) Uani d . 1 1
C C7 0.1582(6) 0.5291(6) 0.2780(3) 0.124(3) Uani d . 1 1
H H7A 0.1317 0.4630 0.2604 0.186 Uiso calc R 1 1
H H7B 0.2230 0.5622 0.2535 0.186 Uiso calc R 1 1
H H7C 0.0844 0.5755 0.2814 0.186 Uiso calc R 1 1
C C8 0.1916(6) 0.5507(5) 0.4913(2) 0.111(2) Uani d . 1 1
H H8A 0.1229 0.6023 0.4903 0.166 Uiso calc R 1 1
H H8B 0.2662 0.5808 0.5106 0.166 Uiso calc R 1 1
H H8C 0.1632 0.4888 0.5127 0.166 Uiso calc R 1 1
Fe Fe1 0.53140(7) 0.75129(5) 0.36820(3) 0.0621(3) Uani d . 1 1
Cl Cl1 0.40700(15) 0.76662(12) 0.44622(6) 0.0934(5) Uani d . 1 1
Cl Cl2 0.6707(2) 0.62448(18) 0.38165(8) 0.1478(9) Uani d . 1 1
Cl Cl3 0.63300(15) 0.90130(13) 0.35368(7) 0.0997(5) Uani d . 1 1
Cl Cl4 0.40818(16) 0.71994(13) 0.29142(6) 0.1007(5) Uani d . 1 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
N1 0.089(3) 0.084(3) 0.108(4) -0.025(3) -0.029(3) 0.027(3)
N2 0.086(3) 0.079(3) 0.107(4) -0.005(3) -0.020(3) 0.016(3)
N3 0.094(3) 0.083(3) 0.097(3) -0.019(3) 0.010(3) -0.012(3)
C1 0.064(3) 0.070(3) 0.060(3) -0.009(2) 0.001(2) 0.004(2)
C2 0.105(4) 0.108(4) 0.064(3) -0.027(4) -0.012(3) 0.008(3)
C3 0.100(4) 0.116(5) 0.080(4) 0.019(4) -0.001(3) 0.007(4)
C4 0.097(4) 0.127(5) 0.083(4) 0.001(4) 0.002(3) -0.012(4)
C5 0.105(4) 0.108(4) 0.050(3) -0.030(3) 0.009(3) -0.009(3)
C6 0.089(4) 0.087(4) 0.071(3) -0.036(3) -0.003(3) 0.003(3)
C7 0.127(5) 0.136(6) 0.110(5) -0.039(4) -0.062(4) 0.046(4)
C8 0.130(5) 0.109(5) 0.093(4) -0.037(4) 0.042(4) -0.043(4)
Fe1 0.0725(5) 0.0589(5) 0.0548(4) 0.0043(3) 0.0006(3) 0.0041(3)
Cl1 0.1005(10) 0.1047(11) 0.0749(9) 0.0156(8) 0.0246(8) 0.0135(7)
Cl2 0.1852(19) 0.1443(18) 0.1138(14) 0.1036(16) 0.0155(12) 0.0183(11)
Cl3 0.1123(11) 0.1022(11) 0.0847(10) -0.0438(9) -0.0079(8) 0.0060(8)
Cl4 0.1173(11) 0.1100(11) 0.0748(9) -0.0393(9) -0.0193(8) 0.0016(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'
Fe Fe 0.3463 0.8444 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C6 N1 N2 112.9(5)
C6 N1 C7 128.6(6)
N2 N1 C7 118.5(5)
N3 N2 N1 102.2(4)
N2 N3 C1 113.1(5)
N2 N3 C8 119.1(5)
C1 N3 C8 127.9(5)
N3 C1 C6 106.1(5)
N3 C1 C2 131.0(5)
C6 C1 C2 122.9(5)
C3 C2 C1 113.9(5)
C3 C2 H2 123.0
C1 C2 H2 123.0
C4 C3 C2 122.7(5)
C4 C3 H3 118.6
C2 C3 H3 118.6
C3 C4 C5 122.4(6)
C3 C4 H4 118.8
C5 C4 H4 118.8
C6 C5 C4 115.1(5)
C6 C5 H5 122.4
C4 C5 H5 122.4
N1 C6 C5 131.3(6)
N1 C6 C1 105.8(5)
C5 C6 C1 122.9(6)
N1 C7 H7A 109.5
N1 C7 H7B 109.5
H7A C7 H7B 109.5
N1 C7 H7C 109.5
H7A C7 H7C 109.5
H7B C7 H7C 109.5
N3 C8 H8A 109.5
N3 C8 H8B 109.5
H8A C8 H8B 109.5
N3 C8 H8C 109.5
H8A C8 H8C 109.5
H8B C8 H8C 109.5
Cl2 Fe1 Cl3 109.81(10)
Cl2 Fe1 Cl4 111.32(8)
Cl3 Fe1 Cl4 108.36(6)
Cl2 Fe1 Cl1 109.85(7)
Cl3 Fe1 Cl1 109.04(7)
Cl4 Fe1 Cl1 108.41(7)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1 C6 1.332(7)
N1 N2 1.390(7)
N1 C7 1.485(7)
N2 N3 1.327(6)
N3 C1 1.367(6)
N3 C8 1.460(6)
C1 C6 1.373(7)
C1 C2 1.390(7)
C2 C3 1.390(8)
C2 H2 0.9300
C3 C4 1.351(8)
C3 H3 0.9300
C4 C5 1.408(8)
C4 H4 0.9300
C5 C6 1.342(7)
C5 H5 0.9300
C7 H7A 0.9600
C7 H7B 0.9600
C7 H7C 0.9600
C8 H8A 0.9600
C8 H8B 0.9600
C8 H8C 0.9600
Fe1 Cl2 2.1636(17)
Fe1 Cl3 2.1786(15)
Fe1 Cl4 2.1840(14)
Fe1 Cl1 2.1867(15)
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
C6 N1 N2 N3 -1.1(5)
C7 N1 N2 N3 179.0(4)
N1 N2 N3 C1 0.9(5)
N1 N2 N3 C8 -177.7(4)
N2 N3 C1 C6 -0.4(5)
C8 N3 C1 C6 178.0(5)
N2 N3 C1 C2 -179.8(5)
C8 N3 C1 C2 -1.4(8)
N3 C1 C2 C3 180.0(5)
C6 C1 C2 C3 0.7(7)
C1 C2 C3 C4 0.1(8)
C2 C3 C4 C5 -1.1(9)
C3 C4 C5 C6 1.3(8)
N2 N1 C6 C5 -179.6(5)
C7 N1 C6 C5 0.4(9)
N2 N1 C6 C1 0.9(5)
C7 N1 C6 C1 -179.2(5)
C4 C5 C6 N1 180.0(5)
C4 C5 C6 C1 -0.6(7)
N3 C1 C6 N1 -0.3(5)
C2 C1 C6 N1 179.2(5)
N3 C1 C6 C5 -179.9(5)
C2 C1 C6 C5 -0.4(7)
