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#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/01/4310194.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_4310194
loop_
_publ_author_name
'Yann Garcia'
'Georges Bravic'
'Christine Gieck'
'Daniel Chasseau'
'Wolfgang Tremel'
'Philipp Gütlich'
_publ_section_title
;
Crystal Structure, Magnetic Properties, and 57Fe Mössbauer Spectroscopy of
the Two-Dimensional Coordination Polymers
[M(1,2-bis(1,2,4-triazol-4-yl)ethane)2(NCS)2] (MII= Fe, Co)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9723
_journal_page_last               9730
_journal_paper_doi               10.1021/ic050971l
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C7 H8 Fe0.5 N7 S'
_chemical_formula_weight         250.2
_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'
_cell_angle_alpha                90
_cell_angle_beta                 90.88
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.439
_cell_length_b                   8.941
_cell_length_c                   9.321
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295(1)
_cell_measurement_theta_max      16.0
_cell_measurement_theta_min      11.5
_cell_volume                     1036.532
_computing_cell_refinement       'CAD-4 (Enraf Nonius,1989)'
_computing_data_collection       'CAD-4 (Enraf Nonius,1989)'
_computing_structure_solution    'MITHRIL (Gilmore, 1984)'
_diffrn_ambient_temperature      295(1)
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       'ω/θ scans'
_diffrn_radiation_detector       counter
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.009
_diffrn_reflns_av_sigmaI/netI    0.017
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            6528
_diffrn_reflns_theta_max         38
_diffrn_reflns_theta_min         2.7
_exptl_absorpt_coefficient_mu    0.978
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.864
_exptl_absorpt_correction_type   'from psi scans'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       prism
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.20
_refine_ls_goodness_of_fit_all   0.832
_refine_ls_goodness_of_fit_gt    0.918
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     143
_refine_ls_number_reflns         5628
_refine_ls_R_factor_all          0.066
_refine_ls_R_factor_gt           0.036
_refine_ls_shift/esd_max         0.223
_refine_ls_shift/esd_mean        0.093
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;                                                                               
 'calc w=1/[σ²(Fo²)+(0.030P)²] where P=(Fo²+2Fc²)/3'                 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.123
_refine_ls_wR_factor_gt          0.097
_reflns_limit_h_max              21
_reflns_limit_h_min              -21
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                3788
_reflns_number_total             5635
_reflns_threshold_expression     I>3σ(I)
_cod_data_source_file            ic050971lsi20051006_113124.cif
_cod_data_source_block           ed:
_cod_original_cell_volume        1036.5
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'H8 C7 N7 S Fe0.5'
_cod_database_code               4310194
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_B_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.5000 0.5000 1.940(4) Bani 1 2 d . . .
S2 S 0.12440(2) 0.57944(4) 0.44562(4) 4.22(1) Bani 1 4 d . . .
C3 C 0.25280(7) 0.55668(9) 0.42790(9) 2.52(2) Bani 1 4 d . . .
N4 N 0.34464(7) 0.5400(1) 0.4139(1) 3.20(3) Bani 1 4 d . . .
N11 N 0.54692(6) 0.73380(7) 0.46876(8) 2.64(2) Bani 1 4 d . . .
N12 N 0.53453(8) 0.81205(8) 0.34203(9) 2.98(3) Bani 1 4 d . . .
C13 C 0.58814(9) 0.93629(8) 0.3593(1) 3.00(3) Bani 1 4 d . . .
N14 N 0.63481(6) 0.94354(7) 0.49105(8) 2.57(2) Bani 1 4 d . . .
C15 C 0.60560(8) 0.81470(9) 0.55602(9) 2.90(3) Bani 1 4 d . . .
C16 C 0.70637(8) 1.05970(9) 0.5478(1) 2.98(3) Bani 1 4 d . . .
N21 N 0.93157(6) 0.94186(8) 0.21458(7) 2.54(2) Bani 1 4 d . . .
N22 N 0.9025(1) 0.79807(9) 0.2506(1) 3.83(3) Bani 1 4 d . . .
C23 C 0.8626(1) 0.8060(1) 0.3796(1) 3.80(4) Bani 1 4 d . . .
N24 N 0.86316(6) 0.94842(8) 0.42866(7) 2.43(2) Bani 1 4 d . . .
C25 C 0.90687(8) 1.0288(1) 0.3219(1) 2.89(3) Bani 1 4 d . . .
C26 C 0.82081(7) 1.0036(1) 0.56394(8) 2.93(2) Bani 1 4 d . . .
H131 H 0.6048 1.0150 0.2976 3 Biso 1 4 c C13 . .
H151 H 0.6446 0.7766 0.6625 3 Biso 1 4 c C15 . .
H231 H 0.8163 0.7217 0.4122 3 Biso 1 4 c C23 . .
H251 H 0.9126 1.1532 0.3314 3 Biso 1 4 c C25 . .
H161 H 0.6961 1.1360 0.4679 3 Biso 1 4 c C16 . .
H162 H 0.6728 1.0919 0.6345 3 Biso 1 4 c C16 . .
H261 H 0.8311 0.9279 0.6410 3 Biso 1 4 c C26 . .
H262 H 0.8702 1.0936 0.5899 3 Biso 1 4 c C26 . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.000 0.000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.002 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.004 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.110 0.124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.301 0.845 '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
_geom_angle_publ_flag
N4 Fe1 N11 91.83(3) . . ?
S2 C3 N4 179.37(9) . . ?
Fe1 N4 C3 151.05(8) . . ?
Fe1 N11 N12 124.83(6) . . ?
Fe1 N11 C15 126.46(6) . . ?
N12 N11 C15 107.88(7) . . ?
N11 N12 C13 106.03(8) . . ?
N12 C13 N14 111.38(8) . . ?
C13 N14 C15 104.54(7) . . ?
C13 N14 C16 127.84(7) . . ?
C15 N14 C16 127.51(7) . . ?
N11 C15 N14 110.16(8) . . ?
N14 C16 C26 111.52(7) . . ?
N22 N21 C25 107.61(8) . . ?
N21 N22 C23 106.12(9) . . ?
N22 C23 N24 111.2(1) . . ?
C23 N24 C25 104.61(8) . . ?
C23 N24 C26 127.58(8) . . ?
C25 N24 C26 127.74(7) . . ?
N21 C25 N24 110.48(8) . . ?
C16 C26 N24 112.16(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N4 2.1116(9) . ?
Fe1 N11 2.1910(7) . ?
S2 C3 1.6210(9) . ?
C3 N4 1.161(1) . ?
N11 N12 1.379(1) . ?
N11 C15 1.304(1) . ?
N12 C13 1.304(1) . ?
C13 N14 1.352(1) . ?
C13 N14 3.303(1) 3_676 ?
C13 C15 3.383(1) 3_676 ?
N14 C15 1.354(1) . ?
N14 C16 1.462(1) . ?
C16 C26 1.515(1) . ?
N21 N22 1.378(1) . ?
N21 C25 1.307(1) . ?
N22 C23 1.310(2) . ?
C23 N24 1.353(1) . ?
N24 C25 1.349(1) . ?
N24 C26 1.460(1) . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N11 Fe1 N4 C3 -105.5(1) . . . . ?
N4 Fe1 N11 N12 -50.74(6) . . . . ?
N4 Fe1 N11 C15 140.98(7) . . . . ?
Fe1 N11 N12 C13 -169.30(6) . . . . ?
C15 N11 N12 C13 0.82(8) . . . . ?
Fe1 N11 C15 N14 168.72(6) . . . . ?
N12 N11 C15 N14 -1.19(7) . . . . ?
N12 C13 N14 C15 -0.55(8) . . . . ?
N12 C13 N14 C16 175.97(8) . . . . ?
C13 N14 C15 N11 1.07(7) . . . . ?
C16 N14 C15 N11 -175.46(8) . . . . ?
C13 N14 C16 C26 -109.00(8) . . . . ?
C15 N14 C16 C26 66.75(8) . . . . ?
N14 C16 C26 N24 57.32(7) . . . . ?
N22 C23 N24 C25 -0.43(9) . . . . ?
N22 C23 N24 C26 176.76(9) . . . . ?
C23 N24 C25 N21 -0.03(8) . . . . ?
C26 N24 C25 N21 -177.22(8) . . . . ?
C23 N24 C26 C16 -93.76(9) . . . . ?
C25 N24 C26 C16 82.81(8) . . . . ?
