# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2009

data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Guo-Cong Guo'
'Li-Zhen Cai'
'Sheng-Ping Guo'
'Jin-Shun Huang'
'Ming-Sheng Wang'
'Hui-Yi Zeng'
'Jian-Ping Zou'

_publ_contact_author_name        'Guo-Cong Guo'
_publ_contact_author_email       GCGUO@FJIRSM.AC.CN

_publ_section_title              
;
A Facile Approach to Hexanary Chalcogenoborate
Featuring 3-D Chiral Honeycomb-Like Open-Framework Constructed
>From Rare-Earth Consolidating Thiogallate-Closo-Dodecaborate
;

# Attachment 'compound_1.CIF'

data_h
_database_code_depnum_ccdc_archive 'CCDC 725683'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
K3ISmGa3B12S12
;
_chemical_name_common            K3ISmGa3B12S12
_chemical_melting_point          ?
_chemical_formula_moiety         K3ISmGa3B12S12
_chemical_formula_sum            'B12 Ga3 I K3 S12 Sm'
_chemical_formula_weight         1118.15

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
B B 0.0013 0.0007 '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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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'
Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   P6(3)22

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'

_cell_length_a                   12.9213(16)
_cell_length_b                   12.9213(16)
_cell_length_c                   9.3181(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     1347.3(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.756
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1034
_exptl_absorpt_coefficient_mu    7.651
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.7562
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'Sphere (Rigaku CrystalClear)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'rotating-anode generator'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku Scxmini CCD'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8983
_diffrn_reflns_av_R_equivalents  0.1070
_diffrn_reflns_av_sigmaI/netI    0.0883
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         25.48
_reflns_number_total             842
_reflns_number_gt                674
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Corp., 2002)'
_computing_cell_refinement       'CrystalClear (Rigaku Corp., 2002)'
_computing_data_reduction        'CrystalClear (Rigaku Corp., 2002)'
_computing_structure_solution    'Siemens SHELXTL^TM^ 5'
_computing_structure_refinement  'Siemens SHELXTL^TM^ 5'
_computing_molecular_graphics    ?
_computing_publication_material  'Siemens SHELXTL^TM^ 5'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(6)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         842
_refine_ls_number_parameters     52
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0427
_refine_ls_wR_factor_ref         0.0926
_refine_ls_wR_factor_gt          0.0856
_refine_ls_goodness_of_fit_ref   0.946
_refine_ls_restrained_S_all      0.970
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sm1 Sm 0.3333 0.6667 0.2500 0.02453(9) Uani 1 6 d S . .
I1 I 0.0000 0.0000 0.7500 0.0767(3) Uani 1 6 d S . .
Ga1 Ga 0.0000 0.53817(4) 0.5000 0.02125(11) Uani 1 2 d S . .
K1 K 0.0000 0.21493(13) 0.5000 0.0989(6) Uani 1 2 d SU . .
S1 S 0.06452(6) 0.67153(7) 0.67950(7) 0.0216(2) Uani 1 1 d . . .
S2 S 0.15916(6) 0.50666(6) 0.44589(7) 0.0178(2) Uani 1 1 d . . .
B1 B 0.2034(2) 0.6676(3) 0.7168(3) 0.0184(10) Uani 1 1 d . . .
B2 B 0.2504(3) 0.5879(3) 0.6062(3) 0.0121(9) Uani 1 1 d . . .

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
Sm1 0.02678(12) 0.02678(12) 0.02004(16) 0.000 0.000 0.01339(6)
I1 0.0695(3) 0.0695(3) 0.0909(5) 0.000 0.000 0.03476(15)
Ga1 0.0208(2) 0.02573(18) 0.01557(19) -0.00149(12) -0.0030(2) 0.01039(12)
K1 0.1500(14) 0.0718(7) 0.1009(10) 0.0139(6) 0.0277(12) 0.0750(7)
S1 0.0191(3) 0.0300(3) 0.0179(3) -0.0063(3) -0.0039(3) 0.0139(2)
S2 0.0162(3) 0.0241(3) 0.0115(3) -0.0028(3) -0.0024(3) 0.0088(2)
B1 0.0116(12) 0.0241(15) 0.0122(14) -0.0090(14) -0.0041(11) 0.0034(11)
B2 0.0164(12) 0.0086(11) 0.0107(13) 0.0018(12) 0.0025(13) 0.0058(8)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

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
Sm1 S2 2.8317(7) 12_565 ?
Sm1 S2 2.8317(7) 3_565 ?
Sm1 S2 2.8317(7) . ?
Sm1 S2 2.8317(7) 10_665 ?
Sm1 S2 2.8317(7) 2_665 ?
Sm1 S2 2.8317(7) 11 ?
I1 K1 3.6249(14) 2 ?
I1 K1 3.6249(14) 5 ?
I1 K1 3.6249(14) 6 ?
I1 K1 3.6249(14) 4 ?
I1 K1 3.6249(14) 3 ?
I1 K1 3.6249(13) . ?
Ga1 S1 2.2417(8) . ?
Ga1 S1 2.2417(8) 9_556 ?
Ga1 S2 2.3424(10) 9_556 ?
Ga1 S2 2.3424(10) . ?
K1 S2 3.3076(16) . ?
K1 S2 3.3076(16) 9_556 ?
K1 S1 3.6040(13) 12_566 ?
K1 S1 3.6040(13) 4_564 ?
K1 I1 3.6249(13) 4_554 ?
K1 K1 4.810(3) 2 ?
K1 K1 4.810(3) 3 ?
S1 B1 1.853(4) . ?
S1 K1 3.6040(13) 4_565 ?
S2 B2 1.867(3) . ?
B1 B2 1.765(6) . ?
B1 B2 1.770(4) 12_566 ?
B1 B1 1.777(5) 10_666 ?
B1 B1 1.813(8) 12_566 ?
B1 B2 1.830(5) 3_565 ?
B2 B1 1.770(4) 12_566 ?
B2 B2 1.811(4) 2_665 ?
B2 B2 1.811(4) 3_565 ?
B2 B1 1.830(5) 2_665 ?

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
S2 Sm1 S2 101.56(3) 12_565 3_565 ?
S2 Sm1 S2 93.01(3) 12_565 . ?
S2 Sm1 S2 82.92(2) 3_565 . ?
S2 Sm1 S2 82.92(2) 12_565 10_665 ?
S2 Sm1 S2 93.01(3) 3_565 10_665 ?
S2 Sm1 S2 173.58(4) . 10_665 ?
S2 Sm1 S2 173.58(4) 12_565 2_665 ?
S2 Sm1 S2 82.92(2) 3_565 2_665 ?
S2 Sm1 S2 82.92(2) . 2_665 ?
S2 Sm1 S2 101.56(3) 10_665 2_665 ?
S2 Sm1 S2 82.92(2) 12_565 11 ?
S2 Sm1 S2 173.58(4) 3_565 11 ?
S2 Sm1 S2 101.56(3) . 11 ?
S2 Sm1 S2 82.92(2) 10_665 11 ?
S2 Sm1 S2 93.01(3) 2_665 11 ?
K1 I1 K1 180.0 2 5 ?
K1 I1 K1 96.86(3) 2 6 ?
K1 I1 K1 83.14(3) 5 6 ?
K1 I1 K1 96.86(3) 2 4 ?
K1 I1 K1 83.14(3) 5 4 ?
K1 I1 K1 83.14(3) 6 4 ?
K1 I1 K1 83.14(3) 2 3 ?
K1 I1 K1 96.86(3) 5 3 ?
K1 I1 K1 180.0 6 3 ?
K1 I1 K1 96.86(3) 4 3 ?
K1 I1 K1 83.14(3) 2 . ?
K1 I1 K1 96.86(3) 5 . ?
K1 I1 K1 96.86(3) 6 . ?
K1 I1 K1 180.0 4 . ?
K1 I1 K1 83.14(3) 3 . ?
S1 Ga1 S1 108.72(5) . 9_556 ?
S1 Ga1 S2 116.19(2) . 9_556 ?
S1 Ga1 S2 105.83(3) 9_556 9_556 ?
S1 Ga1 S2 105.83(3) . . ?
S1 Ga1 S2 116.19(2) 9_556 . ?
S2 Ga1 S2 104.41(4) 9_556 . ?
S2 K1 S2 68.06(5) . 9_556 ?
S2 K1 S1 65.50(3) . 12_566 ?
S2 K1 S1 63.15(3) 9_556 12_566 ?
S2 K1 S1 63.15(3) . 4_564 ?
S2 K1 S1 65.50(3) 9_556 4_564 ?
S1 K1 S1 116.97(5) 12_566 4_564 ?
S2 K1 I1 122.479(15) . 4_554 ?
S2 K1 I1 137.132(14) 9_556 4_554 ?
S1 K1 I1 158.91(4) 12_566 4_554 ?
S1 K1 I1 82.413(19) 4_564 4_554 ?
S2 K1 I1 137.132(14) . . ?
S2 K1 I1 122.479(15) 9_556 . ?
S1 K1 I1 82.413(19) 12_566 . ?
S1 K1 I1 158.91(4) 4_564 . ?
I1 K1 I1 79.98(4) 4_554 . ?
S2 K1 K1 170.732(15) . 2 ?
S2 K1 K1 116.65(2) 9_556 2 ?
S1 K1 K1 123.56(2) 12_566 2 ?
S1 K1 K1 110.64(2) 4_564 2 ?
I1 K1 K1 48.432(14) 4_554 2 ?
I1 K1 K1 48.432(14) . 2 ?
S2 K1 K1 116.65(2) . 3 ?
S2 K1 K1 170.732(15) 9_556 3 ?
S1 K1 K1 110.64(2) 12_566 3 ?
S1 K1 K1 123.56(2) 4_564 3 ?
I1 K1 K1 48.432(14) 4_554 3 ?
I1 K1 K1 48.432(14) . 3 ?
K1 K1 K1 60.0 2 3 ?
B1 S1 Ga1 96.43(11) . . ?
B1 S1 K1 106.26(10) . 4_565 ?
Ga1 S1 K1 149.13(3) . 4_565 ?
B2 S2 Ga1 95.31(13) . . ?
B2 S2 Sm1 93.27(9) . . ?
Ga1 S2 Sm1 117.27(3) . . ?
B2 S2 K1 112.15(10) . . ?
Ga1 S2 K1 93.77(3) . . ?
Sm1 S2 K1 138.13(3) . . ?
B2 B1 B2 107.3(3) . 12_566 ?
B2 B1 B1 108.40(16) . 10_666 ?
B2 B1 B1 62.1(2) 12_566 10_666 ?
B2 B1 B1 59.3(2) . 12_566 ?
B2 B1 B1 59.0(2) 12_566 12_566 ?
B1 B1 B1 108.75(18) 10_666 12_566 ?
B2 B1 B2 60.4(2) . 3_565 ?
B2 B1 B2 107.6(2) 12_566 3_565 ?
B1 B1 B2 58.76(18) 10_666 3_565 ?
B1 B1 B2 106.9(2) 12_566 3_565 ?
B2 B1 S1 121.78(19) . . ?
B2 B1 S1 122.0(2) 12_566 . ?
B1 B1 S1 120.43(11) 10_666 . ?
B1 B1 S1 123.00(11) 12_566 . ?
B2 B1 S1 121.9(2) 3_565 . ?
B1 B2 B1 61.7(3) . 12_566 ?
B1 B2 B2 109.35(19) . 2_665 ?
B1 B2 B2 106.70(18) 12_566 2_665 ?
B1 B2 B2 61.6(2) . 3_565 ?
B1 B2 B2 109.64(19) 12_566 3_565 ?
B2 B2 B2 60.000(1) 2_665 3_565 ?
B1 B2 B1 108.5(2) . 2_665 ?
B1 B2 B1 59.1(2) 12_566 2_665 ?
B2 B2 B1 58.0(2) 2_665 2_665 ?
B2 B2 B1 106.5(2) 3_565 2_665 ?
B1 B2 S2 119.4(2) . . ?
B1 B2 S2 122.10(19) 12_566 . ?
B2 B2 S2 122.37(17) 2_665 . ?
B2 B2 S2 120.15(18) 3_565 . ?
B1 B2 S2 124.2(2) 2_665 . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        25.48
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.706
_refine_diff_density_min         -1.540
_refine_diff_density_rms         0.164