Supplementary Material (ESI) for New Journal of Chemistry
This journal is (c) The Royal Society of Chemistry and 
The Centre National de la Recherche Scientifique, 2006


data_global
_journal_coden_Cambridge         440
# SUBMISSION DETAILS

loop_
_publ_author_name
'Sebastien Floquet'
'Marie-Laure Boillot'
'Nathalie Guillou'
'Philippe Negrier'
'Eric Riviere'

_publ_contact_author_name        'Sebastien Floquet'
#Boillot Marie-Laure

_publ_contact_author_address     
;
S\'ebastien Floquet
Institut Lavoisier de Versailles, UMR 8180
Universit\'e de Versailles
45, Avenue des Etats-Unis
F-78035 Versailles
;

#Boillot Marie-Laure
#ICMMO, Equipe de Chimie Inorganique, UMR 8182
#Universit\'e de Paris Sud
#F-91400 Orsay

_publ_contact_author_email       
sebastien.floquet@uvsq.fr #mboillot@icmo.u-psud.fr
_publ_contact_author_fax         '33 1 39 25 43 81'
_publ_contact_author_phone       '33 1 39 25 43 83'

_publ_requested_journal          'New Journal of Chemistry'
_publ_section_title              
;
The crystallographic phase transition
for a ferric thiosemicarbazone spin crossover complex
studied by X-Ray powder diffraction
;
#=============================================================================
data_373K
_database_code_depnum_ccdc_archive 'CCDC 617382'

#CHEMICAL DATA

_chemical_name_systematic        
; ?
;
#_chemical_formula_ ?
_chemical_formula_weight         625.05

loop_
_atom_type_symbol
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
fe 11.76950 4.76110 7.35730 0.30720 3.52220 15.35350 2.30450 76.88050 1.03690
-1.17900 3.20400
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
br 17.17890 2.17230 5.23580 16.57960 5.63770 0.26090 3.98510 41.43280 2.95570
-0.76700 1.28300
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
s 6.90530 1.46790 5.20340 22.21510 1.43790 0.25360 1.58630 56.17200 0.86690
0.31900 0.55700
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
o 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080
0.04700 0.03200
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560
0.01700 0.00900
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
n 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900
0.02900 0.01800
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5

#=============================================================================

# POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/C'
_symmetry_space_group_name_Hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz #<--must include 'x,y,z'
x,y,z
-x,y+1/2,-z+1/2
-x,-y,-z
x,-y+1/2,z+1/2

_cell_length_a                   21.554(1)
_cell_length_b                   11.4790(5)
_cell_length_c                   8.9428(4)
_cell_angle_alpha                90.00000
_cell_angle_beta                 101.235(2)
_cell_angle_gamma                90.00000
_cell_volume                     2170.2(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    373

_pd_spec_mounting                'glass capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder

#=============================================================================

# EXPERIMENTAL DATA

_diffrn_source                   'X-ray tube'
_diffrn_radiation_type           X-ray
_diffrn_source_target            Cu

_diffrn_radiation_monochromator  Quartz
_diffrn_measurement_device_type  'INEL CPS 120'

# The following four items give details of the measured (not processed)
# powder pattern. Angles are in degrees.

_pd_meas_number_of_points        3030
_pd_meas_2theta_range_min        2.16600
_pd_meas_2theta_range_max        90.00000
_pd_meas_2theta_range_inc        0.029000

#=============================================================================

# REFINEMENT DATA

# The next three items are given as text.

_pd_proc_ls_profile_function     Pseudo-Voigt
_pd_proc_ls_background_function  'background points interpolation'
_pd_proc_ls_pref_orient_corr     'not refined'

# The following profile R-factors are NOT CORRECTED for background
# The sum is extended to all non-excluded points.
# These are the current CIF standard

_pd_proc_ls_prof_R_factor        1.8154
_pd_proc_ls_prof_wR_factor       2.4793
_pd_proc_ls_prof_wR_expected     0.8513

# Items related to LS refinement

_refine_ls_R_I_factor            8.2288
_refine_ls_number_reflns         946
_refine_ls_number_parameters     99
_refine_ls_number_restraints     69

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the
# intensities used in the refinement.

_pd_proc_2theta_range_min        2.1666
_pd_proc_2theta_range_max        70.0000
_pd_proc_2theta_range_inc        0.029000
_pd_proc_wavelength              1.540598

_pd_block_diffractogram_id       ? # The id used for the block containing
# the powder pattern profile (section 11)

# The following items are used to identify the programs used.

_computing_structure_solution    'SIRPOW and FOX'
_computing_structure_refinement  FULLPROF
_computing_molecular_graphics    DIAMOND
#=============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type # Not in version 2.0.1
_atom_site_type_symbol
Fe 0.2479(4) 0.0033(9) 0.0492(10) 0.00000 1.00000 Uiso Fe
Br1 0.0124(4) 0.1776(5) 0.9684(7) 0.00000 1.00000 Uiso Br
S1 -0.3280(8) 0.4558(8) 0.2414(18) 0.00000 1.00000 Uiso S
O1 -0.1973(13) 0.487(3) 0.653(2) 0.00000 1.00000 Uiso O
C11 -0.0501(19) 0.2795(19) 0.861(5) 0.00000 1.00000 Uiso C
C12 -0.057(2) 0.392(2) 0.915(5) 0.00000 1.00000 Uiso C
C13 -0.1059(18) 0.464(2) 0.840(4) 0.00000 1.00000 Uiso C
C14 -0.1464(14) 0.4262(20) 0.705(4) 0.00000 1.00000 Uiso C
C15 -0.1401(15) 0.3106(13) 0.652(4) 0.00000 1.00000 Uiso C
C16 -0.095(2) 0.2360(16) 0.739(5) 0.00000 1.00000 Uiso C
C17 -0.1900(19) 0.2550(14) 0.530(5) 0.00000 1.00000 Uiso C
N12 -0.2761(19) 0.2519(12) 0.330(5) 0.00000 1.00000 Uiso N
C18 -0.320(2) 0.3068(9) 0.234(5) 0.00000 1.00000 Uiso C
N13 -0.3638(18) 0.243(3) 0.132(4) 0.00000 1.00000 Uiso N
N11 -0.2338(18) 0.3158(12) 0.441(4) 0.00000 1.00000 Uiso N
Br2 0.5221(4) 0.1469(6) 0.3796(9) 0.00000 1.00000 Uiso Br
S2 0.1695(7) 0.4544(8) 0.6898(17) 0.00000 1.00000 Uiso S
N21 0.2678(16) 0.3143(13) 0.598(5) 0.00000 1.00000 Uiso N
O2 0.3080(11) 0.470(3) 0.412(3) 0.00000 1.00000 Uiso O
C21 0.4588(19) 0.2484(13) 0.400(7) 0.00000 1.00000 Uiso C
C22 0.4630(8) 0.3674(14) 0.366(7) 0.00000 1.00000 Uiso C
C23 0.4078(13) 0.436(3) 0.348(6) 0.00000 1.00000 Uiso C
C24 0.3587(13) 0.402(2) 0.423(6) 0.00000 1.00000 Uiso C
C25 0.3610(17) 0.288(2) 0.486(7) 0.00000 1.00000 Uiso C
C26 0.4094(18) 0.211(2) 0.470(7) 0.00000 1.00000 Uiso C
C27 0.3088(20) 0.2427(14) 0.560(7) 0.00000 1.00000 Uiso C
N22 0.2286(5) 0.2568(13) 0.6800(12) 0.00000 1.00000 Uiso N
C28 0.1810(15) 0.3068(13) 0.718(4) 0.00000 1.00000 Uiso C
N23 0.153(2) 0.244(3) 0.820(4) 0.00000 1.00000 Uiso N
Ow1 -0.2666(17) 0.009(4) 0.423(4) 0.00000 1.00000 Uiso o

#========================================================================END
data_150K
_database_code_depnum_ccdc_archive 'CCDC 617383'

# CHEMICAL DATA

_chemical_name_systematic        
; ?
;
#_chemical_formula
_chemical_formula_weight         625.05

loop_
_atom_type_symbol
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
fe 11.76950 4.76110 7.35730 0.30720 3.52220 15.35350 2.30450 76.88050 1.03690
-1.17900 3.20400
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
br 17.17890 2.17230 5.23580 16.57960 5.63770 0.26090 3.98510 41.43280 2.95570
-0.76700 1.28300
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
s 6.90530 1.46790 5.20340 22.21510 1.43790 0.25360 1.58630 56.17200 0.86690
0.31900 0.55700
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
c 2.31000 20.84390 1.02000 10.20750 1.58860 0.56870 0.86500 51.65120 0.21560
0.01700 0.00900
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
o 3.04850 13.27710 2.28680 5.70110 1.54630 0.32390 0.86700 32.90890 0.25080
0.04700 0.03200
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
n 12.21260 0.00570 3.13220 9.89330 2.01250 28.99750 1.16630 0.58260 -11.52900
0.02900 0.01800
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5

#=============================================================================

# POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/C'
_symmetry_space_group_name_Hall  '-P 2ybc'

loop_
_symmetry_equiv_pos_as_xyz #<--must include 'x,y,z'
x,y,z
-x,y+1/2,-z+1/2
-x,-y,-z
x,-y+1/2,z+1/2

_cell_length_a                   20.715(2)
_cell_length_b                   11.397(1)
_cell_length_c                   8.8804(7)
_cell_angle_alpha                90.00000
_cell_angle_beta                 90.258(2)
_cell_angle_gamma                90.00000
_cell_volume                     2096.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150

_pd_spec_mounting                'glass capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder

#=============================================================================

# EXPERIMENTAL DATA

_diffrn_source                   'X-ray tube'
_diffrn_radiation_type           X-ray
_diffrn_source_target            Cu

_diffrn_radiation_monochromator  Quartz
_diffrn_measurement_device_type  'INEL CPS 120'

# The following four items give details of the measured (not processed)
# powder pattern. Angles are in degrees.

_pd_meas_number_of_points        2650
_pd_meas_2theta_range_min        3.18100
_pd_meas_2theta_range_max        80.00000
_pd_meas_2theta_range_inc        0.029000

#=============================================================================

# REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
; ?
;

# The next three items are given as text.

_pd_proc_ls_profile_function     Pseudo-Voigt
_pd_proc_ls_background_function  'background points interpolation'
_pd_proc_ls_pref_orient_corr     'not refined'

# The following profile R-factors are NOT CORRECTED for background
# The sum is extended to all non-excluded points.
# These are the current CIF standard

_pd_proc_ls_prof_R_factor        2.1936
_pd_proc_ls_prof_wR_factor       3.0804
_pd_proc_ls_prof_wR_expected     1.0141

# Items related to LS refinement

_refine_ls_R_I_factor            9.4009
_refine_ls_number_reflns         1253
_refine_ls_number_parameters     100
_refine_ls_number_restraints     70

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the
# intensities used in the refinement.

_pd_proc_2theta_range_min        3.1952
_pd_proc_2theta_range_max        79.5000
_pd_proc_2theta_range_inc        0.029000
_pd_proc_wavelength              1.540598

# The following items are used to identify the programs used.

_computing_structure_solution    'SIRPOW and FOX'
_computing_structure_refinement  FULLPROF
_computing_molecular_graphics    DIAMOND

#=============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type # Not in version 2.0.1
_atom_site_type_symbol
Fe 0.2429(5) 0.0050(6) 0.2140(10) 0.00000 1.00000 Uiso Fe
Br1 0.0145(4) 0.1450(6) 0.6531(10) 0.00000 1.00000 Uiso Br
S1 -0.3134(8) 0.4863(11) 0.0948(18) 0.00000 1.00000 Uiso S
C11 -0.0479(17) 0.2547(14) 0.593(5) 0.00000 1.00000 Uiso C
C12 -0.0397(15) 0.3725(15) 0.629(7) 0.00000 1.00000 Uiso C
C13 -0.0903(20) 0.450(3) 0.594(5) 0.00000 1.00000 Uiso C
C14 -0.1346(20) 0.421(2) 0.480(6) 0.00000 1.00000 Uiso C
C15 -0.136(2) 0.3039(16) 0.425(6) 0.00000 1.00000 Uiso C
C16 -0.097(2) 0.2208(18) 0.492(6) 0.00000 1.00000 Uiso C
C17 -0.184(2) 0.264(2) 0.307(6) 0.00000 1.00000 Uiso C
O1 -0.1811(14) 0.494(3) 0.451(3) 0.00000 1.00000 Uiso O
N11 -0.2286(18) 0.3354(14) 0.250(5) 0.00000 1.00000 Uiso N
N12 -0.2724(2) 0.2795(4) 0.1538(6) 0.00000 1.00000 Uiso N
C18 -0.305(2) 0.3391(12) 0.061(5) 0.00000 1.00000 Uiso C
N13 -0.345(2) 0.285(4) -0.030(5) 0.00000 1.00000 Uiso N
Br2 0.5083(4) 0.2380(7) 0.2663(8) 0.00000 1.00000 Uiso Br
S2 0.1654(8) 0.4403(10) 0.878(2) 0.00000 1.00000 Uiso S
C21 0.4513(16) 0.3277(10) 0.379(5) 0.00000 1.00000 Uiso C
C22 0.4506(18) 0.4489(13) 0.365(7) 0.00000 1.00000 Uiso C
C23 0.3993(17) 0.5134(18) 0.426(7) 0.00000 1.00000 Uiso C
C24 0.3491(18) 0.4536(15) 0.494(7) 0.00000 1.00000 Uiso C
C25 0.3564(20) 0.3353(13) 0.527(6) 0.00000 1.00000 Uiso C
C26 0.4003(19) 0.2715(19) 0.446(6) 0.00000 1.00000 Uiso C
C27 0.306(2) 0.2683(18) 0.617(7) 0.00000 1.00000 Uiso C
O2 0.3018(14) 0.513(3) 0.548(3) 0.00000 1.00000 Uiso O
N21 0.2607(19) 0.3242(8) 0.688(6) 0.00000 1.00000 Uiso N
N22 0.222(2) 0.2488(18) 0.767(5) 0.00000 1.00000 Uiso N
C28 0.185(3) 0.2878(14) 0.870(6) 0.00000 1.00000 Uiso C
N23 0.159(3) 0.211(3) 0.958(5) 0.00000 1.00000 Uiso N
Ow1 -0.242(2) -0.015(5) 0.257(5) 0.00000 1.00000 Uiso O

#============================================================END