#------------------------------------------------------------------------------
#$Date: 2019-11-25 01:23:29 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239858 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/03/4350362.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_4350362
loop_
_publ_author_name
'Galet, Ana'
'Gaspar, Ana Belén'
'Muñoz, M Carmen'
'Levchenko, Georgii'
'Real, José Antonio'
_publ_section_title
;
 Pressure effect and crystal structure reinvestigations on the spin
 crossover system: [Fe(bt)2(NCS)2] (bt = 2,2'-bithiazoline) polymorphs A
 and B.
;
_journal_issue                   24
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9670
_journal_page_last               9679
_journal_paper_doi               10.1021/ic060729u
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C14 H16 Fe N6 S6'
_chemical_formula_weight         516.54
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 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                 117.439(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7470(8)
_cell_length_b                   10.7970(5)
_cell_length_c                   11.6000(5)
_cell_measurement_temperature    293(2)
_cell_volume                     2083.83(16)
_computing_cell_refinement       'HKL DENZO'
_computing_data_collection       COLLECT
_computing_data_reduction        'HKL DENZO and SCALEPACK'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0321
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4441
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    1.338
_exptl_crystal_density_diffrn    1.646
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1056
_refine_diff_density_max         0.975
_refine_diff_density_min         -0.606
_refine_diff_density_rms         '0.063 </PRE></BODY></HTML>'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.697
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     124
_refine_ls_number_reflns         2355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.697
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0285
_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)+(0.0582P)²+9.5354P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0713
_refine_ls_wR_factor_ref         0.0784
_reflns_number_gt                2050
_reflns_number_total             2355
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060729usi20060919_022038.cif
_cod_data_source_block           ja275
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4350362
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Fe1 Fe 0.5000 0.34774(4) 0.2500 0.01564(11) Uani 1 2 d S
S1 S 0.67145(3) 0.07086(5) 0.56330(5) 0.02226(13) Uani 1 1 d .
S3 S 0.30784(3) 0.64908(5) 0.23588(6) 0.02947(15) Uani 1 1 d .
S2 S 0.50772(3) 0.14331(5) 0.60580(5) 0.02186(13) Uani 1 1 d .
N2 N 0.48782(10) 0.30498(16) 0.42552(16) 0.0184(3) Uani 1 1 d .
N3 N 0.40902(11) 0.47817(17) 0.20341(18) 0.0239(4) Uani 1 1 d .
N1 N 0.59007(10) 0.20018(16) 0.35157(16) 0.0187(3) Uani 1 1 d .
C4 C 0.53010(11) 0.21297(18) 0.49071(18) 0.0172(4) Uani 1 1 d .
C6 C 0.42916(13) 0.3428(2) 0.4704(2) 0.0239(4) Uani 1 1 d .
H6A H 0.3783 0.3629 0.3962 0.041(3) Uiso 1 1 calc R
H6B H 0.4485 0.4162 0.5243 0.041(3) Uiso 1 1 calc R
C7 C 0.36676(12) 0.54912(19) 0.21735(19) 0.0195(4) Uani 1 1 d .
C3 C 0.65941(13) 0.1535(2) 0.3373(2) 0.0230(4) Uani 1 1 d .
H3A H 0.6983 0.2194 0.3554 0.041(3) Uiso 1 1 calc R
H3B H 0.6418 0.1255 0.2489 0.041(3) Uiso 1 1 calc R
C1 C 0.59312(11) 0.16642(18) 0.45940(19) 0.0167(4) Uani 1 1 d .
C2 C 0.69837(14) 0.0461(2) 0.4317(2) 0.0272(5) Uani 1 1 d .
H2A H 0.7563 0.0472 0.4650 0.041(3) Uiso 1 1 calc R
H2B H 0.6778 -0.0327 0.3892 0.041(3) Uiso 1 1 calc R
C5 C 0.41706(17) 0.2397(2) 0.5471(3) 0.0389(6) Uani 1 1 d .
H5A H 0.3697 0.1916 0.4925 0.041(3) Uiso 1 1 calc R
H5B H 0.4106 0.2728 0.6195 0.041(3) Uiso 1 1 calc R
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'
Fe Fe 0.3463 0.8444 '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
N3 Fe1 N3 94.88(10) 2_655 .
N3 Fe1 N2 87.72(7) 2_655 2_655
N3 Fe1 N2 108.89(7) . 2_655
N3 Fe1 N2 108.89(7) 2_655 .
N3 Fe1 N2 87.72(7) . .
N2 Fe1 N2 155.77(9) 2_655 .
N3 Fe1 N1 162.44(7) 2_655 2_655
N3 Fe1 N1 90.91(7) . 2_655
N2 Fe1 N1 74.72(6) 2_655 2_655
N2 Fe1 N1 87.86(6) . 2_655
N3 Fe1 N1 90.91(7) 2_655 .
N3 Fe1 N1 162.44(7) . .
N2 Fe1 N1 87.86(6) 2_655 .
N2 Fe1 N1 74.72(6) . .
N1 Fe1 N1 88.46(9) 2_655 .
C1 S1 C2 88.74(10) . .
C4 S2 C5 88.86(10) . .
C4 N2 C6 111.48(17) . .
C4 N2 Fe1 114.21(13) . .
C6 N2 Fe1 132.93(13) . .
C7 N3 Fe1 159.45(17) . .
C1 N1 C3 111.61(17) . .
C1 N1 Fe1 113.79(13) . .
C3 N1 Fe1 132.82(13) . .
N2 C4 C1 117.89(17) . .
N2 C4 S2 119.06(15) . .
C1 C4 S2 122.97(15) . .
N2 C6 C5 110.11(17) . .
N2 C6 H6A 109.6 . .
C5 C6 H6A 109.6 . .
N2 C6 H6B 109.6 . .
C5 C6 H6B 109.6 . .
H6A C6 H6B 108.2 . .
N3 C7 S3 179.47(19) . .
N1 C3 C2 109.52(17) . .
N1 C3 H3A 109.8 . .
C2 C3 H3A 109.8 . .
N1 C3 H3B 109.8 . .
C2 C3 H3B 109.8 . .
H3A C3 H3B 108.2 . .
N1 C1 C4 117.64(18) . .
N1 C1 S1 119.24(15) . .
C4 C1 S1 123.11(15) . .
C3 C2 S1 105.17(14) . .
C3 C2 H2A 110.7 . .
S1 C2 H2A 110.7 . .
C3 C2 H2B 110.7 . .
S1 C2 H2B 110.7 . .
H2A C2 H2B 108.8 . .
C6 C5 S2 105.80(16) . .
C6 C5 H5A 110.6 . .
S2 C5 H5A 110.6 . .
C6 C5 H5B 110.6 . .
S2 C5 H5B 110.6 . .
H5A C5 H5B 108.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N3 2.0820(18) 2_655
Fe1 N3 2.0820(18) .
Fe1 N2 2.1998(16) 2_655
Fe1 N2 2.1998(16) .
Fe1 N1 2.2235(17) 2_655
Fe1 N1 2.2235(17) .
S1 C1 1.744(2) .
S1 C2 1.835(2) .
S3 C7 1.628(2) .
S2 C4 1.7436(19) .
S2 C5 1.835(3) .
N2 C4 1.279(3) .
N2 C6 1.475(2) .
N3 C7 1.166(3) .
N1 C1 1.279(3) .
N1 C3 1.473(2) .
C4 C1 1.475(3) .
C6 C5 1.506(3) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C3 C2 1.529(3) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
