#------------------------------------------------------------------------------
#$Date: 2017-11-07 05:29:05 +0200 (Tue, 07 Nov 2017) $
#$Revision: 202879 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/46/7044652.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_7044652
loop_
_publ_author_name
'Gągor, Anna'
'Banach, Grzegorz'
'Węławik, Magdalena'
'Piecha-Bisiorek, Anna'
'Jakubas, Ryszard'
_publ_section_title
;
 The lone-pair-electron-driven phase transition and order-disorder
 processes in thermochromic (2-MIm)SbI4 organic-inorganic hybrid
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C7DT03622A
_journal_year                    2017
_chemical_formula_sum            'C4 H7 I4 N2 Sb'
_chemical_formula_weight         712.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-09-25 deposited with the CCDC.
2017-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.392(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.5504(8)
_cell_length_b                   12.8989(8)
_cell_length_c                   7.8275(4)
_cell_measurement_reflns_used    4279
_cell_measurement_temperature    330(2)
_cell_measurement_theta_max      29.5215
_cell_measurement_theta_min      3.0094
_cell_volume                     1364.11(14)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      330(2)
_diffrn_detector_area_resol_mean 8.4350
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Xcalibur, Sapphire1, long nozzle'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6707
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.677
_diffrn_reflns_theta_min         3.015
_exptl_absorpt_coefficient_mu    11.034
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.42596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    3.469
_exptl_crystal_description       prism
_exptl_crystal_F_000             1232
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.877
_refine_diff_density_min         -1.906
_refine_diff_density_rms         0.118
_refine_ls_extinction_coef       0.00065(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         1298
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.016
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0660P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0911
_refine_ls_wR_factor_ref         0.0940
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1169
_reflns_number_total             1298
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt03622a2.cif
_cod_data_source_block           330K
_cod_database_code               7044652
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_res_file
;

    330K.res created by SHELXL-2014/7


TITL c2c in C2/c
CELL 0.71073 13.550412  12.898945   7.827470    90.0000    94.3921    90.0000
ZERR    4.00   0.0008   0.0008   0.0004   0.000   0.006   0.000
LATT  7
SYMM -X, Y, 0.5-Z
SFAC C H N I Sb
UNIT 16 28 8 16 4
L.S. 20
BOND
FMAP 2
acta
PLAN 50
eqiv $1   -x, -y+1, -z
eqiv $2   -x, y, -z+1/2
eqiv $3   x, -y+1, z+1/2
eqiv $4   -x, y, -z-1/2
flat c1 c2 c3 c4 n1 n2
shel 10 0.82
WGHT    0.066000
EXTI    0.000647
FVAR       0.72044   
MOLE   1
eadp I2 I3
bind Sb I1
SB    5    0.000000    0.405177    0.250000    10.50000    0.04086    0.04018 =
         0.04124    0.00000    0.00672    0.00000
I1    4    0.127413    0.588788    0.084710    11.00000    0.05522    0.06758 =
         0.05877    0.01627   -0.00996   -0.02065
I2    4    0.130798    0.254656    0.133096    11.00000    0.06538    0.09762 =
         0.08044   -0.03834   -0.00114    0.03460


free C1 C4_$4
free C1 C3_$4
free c1 N2_$4
free c1 N1_$4
free c1 C2_$4

free C3 C1_$4
free C3 C2_$4
free C3 C2
free C4 C1_$4
free C4 C2_$4
free C4 C2
free N1 C2_$4
free N1 C1_$4
free N1 N1_$4
free N2 N2_$4
free N2 C2_$4
free N2  C1_$4
C1    1    0.126669    0.079560   -0.317698    10.50000    0.04640    0.12427 =
         0.10922    0.01602    0.01536    0.01202
AFIX 137
H1A   2    0.133848    0.023185   -0.395852    10.50000   -1.50000
H1B   2    0.174679    0.072668   -0.221634    10.50000   -1.50000
H1C   2    0.136841    0.144045   -0.375012    10.50000   -1.50000
AFIX   0
C2    1    0.027221    0.077706   -0.257740    10.50000    0.06068    0.06201 =
         0.06443   -0.00297   -0.02534   -0.00040
C3    1   -0.112168    0.124927   -0.165776    10.50000    0.07933    0.05547 =
         0.08503   -0.00844   -0.02755    0.01303
AFIX  43
H3    2   -0.162353    0.166305   -0.128117    10.50000   -1.20000
AFIX   0
C4    1   -0.113816    0.020551   -0.175898    10.50000    0.10566    0.05771 =
         0.10183   -0.01885   -0.00898    0.01732
AFIX  43
H4    2   -0.164364   -0.023437   -0.147248    10.50000   -1.20000
AFIX   0
N1    3   -0.026412    0.159158   -0.218855    10.50000    0.04855    0.03846 =
         0.11814    0.00598   -0.00801   -0.00216
AFIX  43
H1    2   -0.009071    0.223028   -0.226438    10.50000   -1.20000
AFIX   0
N2    3   -0.027241   -0.006652   -0.235981    10.50000    0.07721    0.03766 =
         0.10695   -0.01416   -0.00951    0.00896
AFIX  43
H2    2   -0.009610   -0.069099   -0.257211    10.50000   -1.20000


AFIX   0
HKLF 4


END
;
_shelx_res_checksum              82414
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sb Sb 0.0000 0.40518(4) 0.2500 0.0406(2) Uani 1 2 d S T P . .
I1 I 0.12741(3) 0.58879(4) 0.08471(6) 0.0613(2) Uani 1 1 d . . . . .
I2 I 0.13080(3) 0.25466(4) 0.13310(6) 0.0815(3) Uani 1 1 d . . . . .
C1 C 0.127(2) 0.080(2) -0.318(3) 0.093(12) Uani 0.5 1 d . . P A 1
H1A H 0.1338 0.0232 -0.3959 0.139 Uiso 0.5 1 calc R U P A 1
H1B H 0.1747 0.0727 -0.2216 0.139 Uiso 0.5 1 calc R U P A 1
H1C H 0.1368 0.1440 -0.3750 0.139 Uiso 0.5 1 calc R U P A 1
C2 C 0.0272(9) 0.0777(10) -0.258(2) 0.064(5) Uani 0.5 1 d . . P A 1
C3 C -0.112(2) 0.1249(18) -0.166(4) 0.075(8) Uani 0.5 1 d . . P A 1
H3 H -0.1624 0.1663 -0.1281 0.090 Uiso 0.5 1 calc R U P A 1
C4 C -0.114(2) 0.0206(16) -0.176(3) 0.089(8) Uani 0.5 1 d . . P A 1
H4 H -0.1644 -0.0234 -0.1472 0.107 Uiso 0.5 1 calc R U P A 1
N1 N -0.0264(8) 0.1592(8) -0.219(2) 0.069(4) Uani 0.5 1 d . . P A 1
H1 H -0.0091 0.2230 -0.2264 0.083 Uiso 0.5 1 calc R U P A 1
N2 N -0.0272(9) -0.0067(8) -0.236(3) 0.075(5) Uani 0.5 1 d . . P A 1
H2 H -0.0096 -0.0691 -0.2572 0.090 Uiso 0.5 1 calc R U P A 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_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Sb 0.0409(4) 0.0402(3) 0.0412(3) 0.000 0.0067(2) 0.000
I1 0.0552(3) 0.0676(4) 0.0588(3) 0.01627(19) -0.0100(2) -0.02065(18)
I2 0.0654(4) 0.0976(5) 0.0804(4) -0.0383(3) -0.0011(3) 0.0346(3)
C1 0.046(11) 0.12(4) 0.109(18) 0.02(2) 0.015(10) 0.01(2)
C2 0.061(14) 0.062(9) 0.064(8) -0.003(8) -0.025(12) 0.000(6)
C3 0.079(19) 0.055(13) 0.085(12) -0.008(10) -0.028(11) 0.013(11)
C4 0.106(17) 0.058(13) 0.102(15) -0.019(12) -0.009(11) 0.017(12)
N1 0.049(10) 0.038(5) 0.118(13) 0.006(6) -0.008(8) -0.002(4)
N2 0.077(14) 0.038(5) 0.107(12) -0.014(7) -0.010(14) 0.009(5)
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 '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
I2 Sb I2 93.28(3) . 2
I2 Sb I1 88.147(14) . 6_566
I2 Sb I1 93.880(16) 2 6_566
I2 Sb I1 93.880(16) . 5_565
I2 Sb I1 88.147(14) 2 5_565
I1 Sb I1 177.05(2) 6_566 5_565
I2 Sb I1 90.360(17) . .
I2 Sb I1 172.903(15) 2 .
I1 Sb I1 92.325(13) 6_566 .
I1 Sb I1 85.527(13) 5_565 .
Sb I1 Sb 94.473(13) 5_565 .
C2 C2 N1 91.7(10) 2_554 2_554
C2 C2 N2 90.6(10) 2_554 2_554
N1 C2 N2 168(3) 2_554 2_554
N1 C2 N1 42.3(12) 2_554 .
N2 C2 N1 143.5(16) 2_554 .
N1 C2 N2 145.9(15) 2_554 .
N1 C2 N2 107.4(12) . .
C2 C2 C1 170(3) 2_554 .
N1 C2 C1 126.6(18) . .
N2 C2 C1 126.0(17) . .
C2 C2 C3 150(2) 2_554 2_554
N2 C2 C3 113.1(18) 2_554 2_554
N1 C2 C3 103.0(14) . 2_554
N2 C2 C3 148.1(19) . 2_554
C2 C2 C4 147.9(16) 2_554 2_554
N1 C2 C4 114.8(16) 2_554 2_554
N1 C2 C4 156.8(15) . 2_554
N1 C3 C4 109(3) . .
N2 C4 C3 106(3) . .
C2 N1 C3 108.3(14) . .
C2 N2 C4 109.8(15) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb I2 2.8278(5) .
Sb I2 2.8279(5) 2
Sb I1 3.0262(5) 6_566
Sb I1 3.0262(5) 5_565
Sb I1 3.2567(6) .
I1 Sb 3.0262(5) 5_565
C1 C2 1.46(3) .
C2 N1 1.326(15) .
C2 N2 1.333(16) .
C3 N1 1.34(3) .
C3 C4 1.35(3) .
C4 N2 1.34(3) .
