#Supplementary Material (ESI) for Chemical Communications
#This journal is (c) The Royal Society of Chemistry 2010
data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Demchenko, Pavlo'
'Gladyshevskii, Roman'
'Volkov, Sergei'
'Yanko, Oleg'
'Kharkova, Lyudmila'
'Fokina, Zoya'
'Fokin, Andrey'

_publ_contact_author_name        'Gladyshevskii, Roman'
_publ_contact_author_email       roman.gladyshevskii@franko.lviv.ua

_publ_section_title              
;
The first nonaselenium ring
;

# Attachment 'Rh2Se9Cl6-prof.cif'
#==============================================
# Powder diffraction pattern number 1
#==============================================
# Attachment 'Rh2Se9Cl6.cif'

##############################################################################
### FullProf-generated CIF output file (version: February 2008) ###
### Template of CIF submission form for structure report ###
##############################################################################

# This file has been generated using FullProf.2k taking one example of
# structure report provided by Acta Cryst. It is given as a 'template' with
# filled structural items. Many other items are left unfilled and it is the
# responsibility of the user to properly fill or suppress them. In principle
# all question marks '?' should be replaced by the appropriate text or
# numerical value depending on the kind of CIF item.
# See the document: cif_core.dic (URL: http://www.iucr.org) for details.

# Please notify any error or suggestion to:
# Juan Rodriguez-Carvajal (jrc@ill.eu)
# Improvements will be progressively added as needed.

#=============================================================================
data_Rh2Se9Cl6
_database_code_depnum_ccdc_archive 'CCDC 768137'
#TrackingRef 'Rh2Se9Cl6.cif'

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

# 5. CHEMICAL DATA

_chemical_name_systematic        
; 'dirhodium nonaselenium hexachloride'
;
_chemical_name_common            'rhodium selenium chloride'
_chemical_name_structure_type    'own structure type'
_chemical_properties_physical    hygroscopic
_chemical_temperature_decomposition 573
_chemical_formula_moiety         'Cl6 Rh2 Se9'
_chemical_formula_structural     '(Rh Cl3)2 Se9'
_chemical_formula_analytical     ?
_chemical_formula_iupac          'Rh2 Se9 Cl6'
_chemical_formula_sum            'Cl6 Rh2 Se9'
_chemical_formula_weight         1129.16
_chemical_melting_point          ?
_chemical_compound_source        ? # for minerals and
# natural products

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
rh 19.29570 0.75154 14.35010 8.21758 4.73425 25.87490 1.28918 98.60620 5.32800
-0.07700 3.60500
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
se 17.00060 2.40980 5.81960 0.27260 3.97310 15.23720 4.35430 43.81630 2.84090
-0.87900 1.13900
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5
cl 11.46040 0.01040 7.19640 1.16620 6.25560 18.51940 1.64550 47.77840 -9.55740
0.34800 0.70200
International_Tables_for_Crystallography_Vol.C(1991)_Tables_6.1.1.4_and_6.1.1.5

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

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'

loop_
_symmetry_equiv_pos_as_xyz #<--must include 'x,y,z'
x,y,z
-y+3/4,x+1/4,z+1/4
-x+1/2,-y,z+1/2
y+3/4,-x+3/4,z+3/4
-x,-y,-z
y+1/4,-x+3/4,-z+3/4
x+1/2,y,-z+1/2
-y+1/4,x+1/4,-z+1/4
x+1/2,y+1/2,z+1/2
-y+1/4,x+3/4,z+3/4
-x,-y+1/2,z
y+1/4,-x+1/4,z+1/4
-x+1/2,-y+1/2,-z+1/2
y+3/4,-x+1/4,-z+1/4
x,y+1/2,-z
-y+3/4,x+3/4,-z+3/4

_cell_length_a                   12.20346(9)
_cell_length_b                   12.20346(9)
_cell_length_c                   23.7125(3)
_cell_angle_alpha                90.00000
_cell_angle_beta                 90.00000
_cell_angle_gamma                90.00000
_cell_volume                     3531.38(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    297(1)
_cell_special_details            
; ?
;
# The next three fields give the specimen dimensions in mm. The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              12 # perpendicular to
# equatorial plane
_pd_spec_size_equat              0.5 # parallel to
# scattering vector
# in transmission
_pd_spec_size_thick              0.25 # parallel to
# scattering vector
# in reflection

# The next six fields are character fields that describe the specimen.

_pd_spec_mount_mode              transmission
_pd_spec_mounting                'glass capillary'
_pd_spec_orientation             vertical
_pd_spec_shape                   cylinder
_pd_char_particle_morphology     'loose powder, size < 0.04 mm'
_pd_char_colour                  orange_red

# The following three fields describe the preparation of the specimen.
# The cooling rate is in K/min. The pressure at which the sample was
# prepared is in kPa. The temperature of preparation is in K.

_pd_prep_cool_rate               ?
_pd_prep_pressure                101.3
_pd_prep_temperature             373

# The next four fields are normally only needed for transmission experiments.

_exptl_absorpt_coefficient_mu    44.52
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?

_exptl_crystal_density_diffrn    4.248
_exptl_crystal_F_000             3984

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

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
;Calibration according to "User^,^s Manual STOE STADI P", standards in use are
NIST SRM640b (Silicon), NIST SRM676 (Al~2~O~3~), LaB~6~, SiO~2~.
;

_diffrn_ambient_environment      vacuum
_diffrn_ambient_temperature      297(1)

_diffrn_detector                 'linear PSD'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'STOE linear PSD'

_diffrn_measurement_device_type  'STOE STADI P'
_diffrn_measurement_method       'data from 2\q scans'

_diffrn_radiation_monochromator  'Ge (111) curved crystal'
_diffrn_radiation_probe          X-ray
_diffrn_radiation_source         'sealed X-ray tube'
_diffrn_radiation_type           'Cu K\a~1~'
_diffrn_radiation_wavelength     1.540598

_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           40
_diffrn_source_details           'Generator Seifert ID3003'
_diffrn_source_power             1.6
_diffrn_source_size              '12 mm x 0.4mm long fine-focus'
_diffrn_source_take-off_angle    6
_diffrn_source_target            Cu
_diffrn_source_type              'STOE PW2773/00'
_diffrn_source_voltage           40

_pd_meas_scan_method             step
_pd_meas_special_details         
; long collimator 0.5 mm
;

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

_pd_meas_number_of_points        6034
_pd_meas_2theta_range_min        3.00000
_pd_meas_2theta_range_max        93.49500
_pd_meas_2theta_range_inc        0.015000

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

# 8. REFINEMENT DATA

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

_pd_proc_ls_special_details      
; Asymmetry correction as in: B\'erar, J.-F.; Baldinozzi, G.
J. Appl.Cryst. 26 (1993) 128-129.
Absorption correction during refinement: FullProf Absorption correction
(muR-eff = 3.55), according to type "Cylinder Debye-Scherrer (Hewat formula)".
;

# The next three items are given as text.

_pd_proc_ls_profile_function     pseudo-Voigt
_pd_proc_ls_background_function  
;Linear interpolation between a set background points with refinable heights.
The background points were determined automatically; the values were refined
to improve the agreement at opening cycles, then were fixed.
;
_pd_proc_ls_pref_orient_corr     
;No significance preferred orientation effect was observed
;

_pd_calc_method                  'Rietveld Refinement'
_pd_proc_ls_peak_cutoff          0.00500

# 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        0.053225
_pd_proc_ls_prof_wR_factor       0.069835
_pd_proc_ls_prof_wR_expected     0.059939

# The following profile R-factors are CORRECTED for background
# The sum is extended to all non-excluded points.
# These items are not in the current CIF standard, but are defined above

#_pd_proc_ls_prof_cR_factor 0.139772
#_pd_proc_ls_prof_cwR_factor 0.150160
#_pd_proc_ls_prof_cwR_expected 0.128881

# The following items are not in the CIF standard, but are defined above

#_pd_proc_ls_prof_chi2 1.3575
#_pd_proc_ls_prof_echi2 1.3604

# Items related to LS refinement

_refine_ls_structure_factor_coef Inet
_refine_ls_matrix_type           fullcycle
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     
;Standard least-square refinement with w=1.0/\s^2^(Y~iobs~)
;
_refine_ls_R_I_factor            0.028175
_refine_ls_number_reflns         833
_refine_ls_number_parameters     83
_refine_ls_number_constraints    1
_refine_ls_number_restraints     0
_refine_ls_shift/su_max          0.0

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   1.1651

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap

# 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        3.0000
_pd_proc_2theta_range_max        93.4950
_pd_proc_2theta_range_inc        0.015000
_pd_proc_wavelength              1.540598

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

_pd_block_diffractogram_id       Rh2Se9Cl6_prof

# Give appropriate details in the next two text fields.

_pd_proc_info_excluded_regions   0
_pd_proc_info_data_reduction     'no reduction'

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

_computing_data_collection       'STOE WinXPOW (Stoe & Cie GmbH, 2007) [1]'
_computing_cell_refinement       'N-TREOR09 (Altomare et al., 2009) [2]'
_computing_structure_solution    'EXPO2009 (Altomare et al., 2004) [3]'
_computing_structure_refinement  'FullProf.2k (Rodriguez-Carvajal, 2001) [4]'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 2001) [7]'
_computing_publication_material  
'enCIFer (CCDC, 2008); publCIF (Westrip, IUCR, 2009)'

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

# 9. 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
Rh1 0.1407(3) 0.1403(3) 0.38981(12) 0.032(2) 1.00000 Uani RH
Se1 0.0078(4) 0.3958(4) 0.32462(17) 0.036(3) 1.00000 Uani SE
Se2 0.0319(4) 0.1572(3) 0.47444(17) 0.039(3) 1.00000 Uani SE
Se3 0.3269(3) 0.1709(4) 0.12904(17) 0.037(3) 1.00000 Uani SE
Se4 0.3571(4) 0.0812(4) 0.04184(16) 0.041(3) 1.00000 Uani SE
Se5 0.00000 0.25000 0.2589(2) 0.036(4) 1.00000 Uani SE
Cl1 0.0964(8) 0.0386(9) 0.2011(4) 0.048(8) 1.00000 Uani CL
Cl2 0.1279(8) 0.0113(7) 0.0658(4) 0.044(8) 1.00000 Uani CL
Cl3 0.3766(7) 0.5526(6) 0.0930(3) 0.028(6) 1.00000 Uani CL

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
_atom_site_aniso_type_symbol
Rh1 0.039(2) 0.023(2) 0.032(2) 0.0116(18) 0.0009(18) -0.0008(17) RH
Se1 0.036(3) 0.032(3) 0.039(3) 0.003(3) 0.012(3) 0.004(3) SE
Se2 0.040(4) 0.023(3) 0.054(3) 0.011(3) 0.011(3) 0.003(3) SE
Se3 0.032(4) 0.042(3) 0.038(3) -0.002(2) 0.004(3) -0.009(3) SE
Se4 0.046(4) 0.031(3) 0.046(3) -0.002(3) 0.009(3) -0.004(3) SE
Se5 0.057(5) 0.031(5) 0.020(4) 0.004(4) 0.00000 0.00000 SE
Cl1 0.042(8) 0.058(8) 0.043(9) -0.016(7) -0.002(6) -0.004(6) CL
Cl2 0.025(7) 0.026(7) 0.081(10) -0.007(5) 0.004(7) -0.029(7) CL
Cl3 0.047(7) 0.022(6) 0.015(6) -0.015(6) 0.010(6) 0.004(5) CL

# Note: if the displacement parameters were refined anisotropically
# the U matrices should be given as for single-crystal studies.

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

# 10. DISTANCES AND ANGLES / MOLECULAR GEOMETRY

_geom_special_details            ?

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
Rh1 Se1 2.422(6) 11_555 yes
Rh1 Se2 2.415(5) . yes
Rh1 Se3 2.380(6) 13_555 yes
Rh1 Cl1 2.323(10) 12_555 yes
Rh1 Cl2 2.301(10) 12_555 yes
Rh1 Cl3 2.398(8) 13_555 yes
Se1 Rh1 2.422(6) 11_555 no
Se1 Se3 2.437(6) 13_555 yes
Se1 Se5 2.367(6) . yes
Se2 Rh1 2.415(5) . no
Se2 Se2 2.395(5) 11_555 yes
Se2 Se4 2.358(7) 7_455 yes
Se3 Rh1 2.380(6) 13_555 no
Se3 Se1 2.437(6) 13_555 no
Se3 Se4 2.368(6) . yes
Se4 Se2 2.358(7) 7_555 no
Se4 Se3 2.368(6) . no
Se5 Se1 2.367(6) . no
Se5 Se1 2.367(6) 11_555 no
Cl1 Rh1 2.323(11) 10_544 no
Cl2 Rh1 2.301(10) 10_544 no
Cl3 Rh1 2.398(8) 13_555 no

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set.
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./