# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry C.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_f:\huangyin\131104hy2\work\t
_database_code_depnum_ccdc_archive 'CCDC 997373'
_audit_update_record             
;
2014-04-15 deposited with the CCDC.
2015-08-13 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Cl3 F2 K2 Sb'
_chemical_formula_weight         344.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P2(1)2(1)2(1)

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

_cell_length_a                   7.6320(11)
_cell_length_b                   8.1788(11)
_cell_length_c                   12.7931(17)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     798.55(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1824
_cell_measurement_theta_min      2.96
_cell_measurement_theta_max      26.39

_exptl_crystal_description       ?
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.864
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             632
_exptl_absorpt_coefficient_mu    5.438
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            6059
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0408
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         28.38
_reflns_number_total             1997
_reflns_number_gt                1848
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² 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/[σ²(Fo²)+(0.0098P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   constr
_refine_ls_hydrogen_treatment    constr
_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   0.01(3)
_refine_ls_number_reflns         1997
_refine_ls_number_parameters     73
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0282
_refine_ls_R_factor_gt           0.0241
_refine_ls_wR_factor_ref         0.0398
_refine_ls_wR_factor_gt          0.0381
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_restrained_S_all      1.013
_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
Cl1 Cl 0.93324(19) -0.16246(13) 0.57768(9) 0.0445(3) Uani 1 1 d . . .
Cl2 Cl 0.76727(15) 0.32504(13) 0.34489(9) 0.0345(3) Uani 1 1 d . . .
Cl3 Cl 0.75116(15) 0.28500(13) 0.65223(8) 0.0314(3) Uani 1 1 d . . .
F1 F 0.8952(4) -0.0291(3) 0.34815(18) 0.0327(6) Uani 1 1 d . . .
F2 F 0.6469(3) 0.0439(3) 0.48150(18) 0.0296(6) Uani 1 1 d . . .
K1 K 0.99281(15) 0.14364(12) 0.14903(8) 0.0395(3) Uani 1 1 d . . .
K2 K 0.96081(13) 0.03343(11) 0.79251(7) 0.0272(2) Uani 1 1 d . . .
Sb1 Sb 0.89165(3) 0.11439(3) 0.473114(19) 0.02045(7) Uani 1 1 d . . .


_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
Cl1 Sb1 2.6490(11) . ?
Cl1 K2 3.0980(14) 3_746 ?
Cl1 K2 3.1881(15) . ?
Cl1 K1 3.3534(16) 3_745 ?
Cl1 K1 3.3808(18) 2_655 ?
Cl2 Sb1 2.5613(11) . ?
Cl2 K2 3.1464(15) 4_456 ?
Cl2 K1 3.1857(15) 3_755 ?
Cl2 K1 3.3827(16) . ?
Cl2 K2 3.4749(15) 2_654 ?
Cl3 Sb1 2.8893(11) . ?
Cl3 K2 3.0757(15) 3_756 ?
Cl3 K2 3.1645(14) . ?
Cl3 K1 3.2699(16) 4_456 ?
F1 Sb1 1.983(2) . ?
F1 K2 2.809(3) 2_654 ?
F1 K1 2.810(2) 3_745 ?
F1 K1 3.007(3) . ?
F2 Sb1 1.958(2) . ?
F2 K2 2.631(2) 2_654 ?
F2 K1 2.843(2) 2_655 ?
K1 F1 2.810(2) 3_755 ?
K1 F2 2.843(2) 2_654 ?
K1 Cl2 3.1857(15) 3_745 ?
K1 Cl3 3.2698(16) 4_556 ?
K1 Cl1 3.3535(16) 3_755 ?
K1 Cl1 3.3808(18) 2_654 ?
K1 K2 4.1776(16) 2_654 ?
K1 K2 4.5048(15) 4_556 ?
K1 K2 4.6557(15) 1_554 ?
K1 K2 4.7806(16) 2_754 ?
K2 F2 2.631(2) 2_655 ?
K2 F1 2.809(3) 2_655 ?
K2 Cl3 3.0758(15) 3_746 ?
K2 Cl1 3.0981(14) 3_756 ?
K2 Cl2 3.1464(15) 4_556 ?
K2 Cl2 3.4749(15) 2_655 ?
K2 Sb1 3.7465(10) 2_655 ?
K2 Sb1 4.1728(11) . ?
K2 K1 4.1776(16) 2_655 ?
K2 K2 4.2736(8) 3_756 ?
Sb1 K2 3.7465(10) 2_654 ?

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
Sb1 Cl1 K2 171.19(6) . 3_746 ?
Sb1 Cl1 K2 90.78(4) . . ?
K2 Cl1 K2 85.65(3) 3_746 . ?
Sb1 Cl1 K1 89.29(4) . 3_745 ?
K2 Cl1 K1 92.29(4) 3_746 3_745 ?
K2 Cl1 K1 166.43(5) . 3_745 ?
Sb1 Cl1 K1 88.98(4) . 2_655 ?
K2 Cl1 K1 98.21(4) 3_746 2_655 ?
K2 Cl1 K1 78.92(4) . 2_655 ?
K1 Cl1 K1 114.64(5) 3_745 2_655 ?
Sb1 Cl2 K2 151.73(5) . 4_456 ?
Sb1 Cl2 K1 108.76(4) . 3_755 ?
K2 Cl2 K1 98.05(4) 4_456 3_755 ?
Sb1 Cl2 K1 89.47(4) . . ?
K2 Cl2 K1 97.23(4) 4_456 . ?
K1 Cl2 K1 94.84(3) 3_755 . ?
Sb1 Cl2 K2 75.03(3) . 2_654 ?
K2 Cl2 K2 80.23(3) 4_456 2_654 ?
K1 Cl2 K2 169.34(5) 3_755 2_654 ?
K1 Cl2 K2 75.05(3) . 2_654 ?
Sb1 Cl3 K2 103.66(4) . 3_756 ?
Sb1 Cl3 K2 87.02(3) . . ?
K2 Cl3 K2 86.43(3) 3_756 . ?
Sb1 Cl3 K1 157.92(4) . 4_456 ?
K2 Cl3 K1 97.72(4) 3_756 4_456 ?
K2 Cl3 K1 88.86(4) . 4_456 ?
Sb1 F1 K2 101.45(10) . 2_654 ?
Sb1 F1 K1 123.88(11) . 3_745 ?
K2 F1 K1 106.59(8) 2_654 3_745 ?
Sb1 F1 K1 114.09(9) . . ?
K2 F1 K1 91.77(8) 2_654 . ?
K1 F1 K1 112.52(8) 3_745 . ?
Sb1 F2 K2 108.57(10) . 2_654 ?
Sb1 F2 K1 123.90(10) . 2_655 ?
K2 F2 K1 116.48(8) 2_654 2_655 ?
F1 K1 F2 129.62(7) 3_755 2_654 ?
F1 K1 F1 120.80(6) 3_755 . ?
F2 K1 F1 106.99(7) 2_654 . ?
F1 K1 Cl2 127.15(7) 3_755 3_745 ?
F2 K1 Cl2 78.03(5) 2_654 3_745 ?
F1 K1 Cl2 74.78(6) . 3_745 ?
F1 K1 Cl3 68.69(6) 3_755 4_556 ?
F2 K1 Cl3 155.30(6) 2_654 4_556 ?
F1 K1 Cl3 64.82(6) . 4_556 ?
Cl2 K1 Cl3 77.32(4) 3_745 4_556 ?
F1 K1 Cl1 60.63(5) 3_755 3_755 ?
F2 K1 Cl1 70.51(5) 2_654 3_755 ?
F1 K1 Cl1 175.33(7) . 3_755 ?
Cl2 K1 Cl1 108.13(4) 3_745 3_755 ?
Cl3 K1 Cl1 119.12(4) 4_556 3_755 ?
F1 K1 Cl1 104.64(7) 3_755 2_654 ?
F2 K1 Cl1 57.35(5) 2_654 2_654 ?
F1 K1 Cl1 90.67(6) . 2_654 ?
Cl2 K1 Cl1 126.63(4) 3_745 2_654 ?
Cl3 K1 Cl1 141.42(4) 4_556 2_654 ?
Cl1 K1 Cl1 84.65(3) 3_755 2_654 ?
F1 K1 Cl2 74.19(6) 3_755 . ?
F2 K1 Cl2 127.18(6) 2_654 . ?
F1 K1 Cl2 56.80(5) . . ?
Cl2 K1 Cl2 129.28(4) 3_745 . ?
Cl3 K1 Cl2 69.67(4) 4_556 . ?
Cl1 K1 Cl2 121.26(4) 3_755 . ?
Cl1 K1 Cl2 71.98(4) 2_654 . ?
F1 K1 K2 125.22(6) 3_755 2_654 ?
F2 K1 K2 80.41(5) 2_654 2_654 ?
F1 K1 K2 42.23(6) . 2_654 ?
Cl2 K1 K2 100.49(4) 3_745 2_654 ?
Cl3 K1 K2 102.71(4) 4_556 2_654 ?
Cl1 K1 K2 133.11(4) 3_755 2_654 ?
Cl1 K1 K2 48.50(3) 2_654 2_654 ?
Cl2 K1 K2 53.48(3) . 2_654 ?
F1 K1 K2 36.70(6) 3_755 4_556 ?
F2 K1 K2 137.63(6) 2_654 4_556 ?
F1 K1 K2 109.35(6) . 4_556 ?
Cl2 K1 K2 91.13(3) 3_745 4_556 ?
Cl3 K1 K2 44.62(3) 4_556 4_556 ?
Cl1 K1 K2 74.51(3) 3_755 4_556 ?
Cl1 K1 K2 141.33(4) 2_654 4_556 ?
Cl2 K1 K2 91.34(3) . 4_556 ?
K2 K1 K2 141.94(3) 2_654 4_556 ?
F1 K1 K2 102.30(6) 3_755 1_554 ?
F2 K1 K2 30.38(5) 2_654 1_554 ?
F1 K1 K2 136.55(5) . 1_554 ?
Cl2 K1 K2 84.01(3) 3_745 1_554 ?
Cl3 K1 K2 145.88(4) 4_556 1_554 ?
Cl1 K1 K2 41.67(2) 3_755 1_554 ?
Cl1 K1 K2 72.17(3) 2_654 1_554 ?
Cl2 K1 K2 141.62(4) . 1_554 ?
K2 K1 K2 108.65(3) 2_654 1_554 ?
K2 K1 K2 108.53(3) 4_556 1_554 ?
F1 K1 K2 91.05(6) 3_755 2_754 ?
F2 K1 K2 116.94(5) 2_654 2_754 ?
F1 K1 K2 75.44(6) . 2_754 ?
Cl2 K1 K2 40.67(3) 3_745 2_754 ?
Cl3 K1 K2 39.61(3) 4_556 2_754 ?
Cl1 K1 K2 109.18(4) 3_755 2_754 ?
Cl1 K1 K2 163.01(4) 2_654 2_754 ?
Cl2 K1 K2 107.00(3) . 2_754 ?
K2 K1 K2 116.69(3) 2_654 2_754 ?
K2 K1 K2 54.709(16) 4_556 2_754 ?
K2 K1 K2 111.30(2) 1_554 2_754 ?
F2 K2 F1 57.45(7) 2_655 2_655 ?
F2 K2 Cl3 81.56(6) 2_655 3_746 ?
F1 K2 Cl3 128.66(6) 2_655 3_746 ?
F2 K2 Cl1 77.41(6) 2_655 3_756 ?
F1 K2 Cl1 97.28(6) 2_655 3_756 ?
Cl3 K2 Cl1 102.74(4) 3_746 3_756 ?
F2 K2 Cl2 146.52(6) 2_655 4_556 ?
F1 K2 Cl2 149.91(6) 2_655 4_556 ?
Cl3 K2 Cl2 80.80(4) 3_746 4_556 ?
Cl1 K2 Cl2 79.05(4) 3_756 4_556 ?
F2 K2 Cl3 121.30(6) 2_655 . ?
F1 K2 Cl3 70.29(5) 2_655 . ?
Cl3 K2 Cl3 157.11(3) 3_746 . ?
Cl1 K2 Cl3 85.06(4) 3_756 . ?
Cl2 K2 Cl3 79.62(4) 4_556 . ?
F2 K2 Cl1 130.60(6) 2_655 . ?
F1 K2 Cl1 98.53(6) 2_655 . ?
Cl3 K2 Cl1 85.03(4) 3_746 . ?
Cl1 K2 Cl1 151.98(4) 3_756 . ?
Cl2 K2 Cl1 75.66(4) 4_556 . ?
Cl3 K2 Cl1 78.73(4) . . ?
F2 K2 Cl2 57.54(5) 2_655 2_655 ?
F1 K2 Cl2 57.04(5) 2_655 2_655 ?
Cl3 K2 Cl2 75.90(4) 3_746 2_655 ?
Cl1 K2 Cl2 134.81(4) 3_756 2_655 ?
Cl2 K2 Cl2 142.23(4) 4_556 2_655 ?
Cl3 K2 Cl2 113.87(4) . 2_655 ?
Cl1 K2 Cl2 73.09(4) . 2_655 ?
F2 K2 Sb1 29.70(5) 2_655 2_655 ?
F1 K2 Sb1 31.26(5) 2_655 2_655 ?
Cl3 K2 Sb1 99.11(3) 3_746 2_655 ?
Cl1 K2 Sb1 96.65(3) 3_756 2_655 ?
Cl2 K2 Sb1 175.54(4) 4_556 2_655 ?
Cl3 K2 Sb1 101.33(3) . 2_655 ?
Cl1 K2 Sb1 108.79(4) . 2_655 ?
Cl2 K2 Sb1 41.33(2) 2_655 2_655 ?
F2 K2 Sb1 153.97(6) 2_655 . ?
F1 K2 Sb1 97.34(5) 2_655 . ?
Cl3 K2 Sb1 114.85(3) 3_746 . ?
Cl1 K2 Sb1 115.50(3) 3_756 . ?
Cl2 K2 Sb1 59.24(3) 4_556 . ?
Cl3 K2 Sb1 43.75(2) . . ?
Cl1 K2 Sb1 39.40(2) . . ?
Cl2 K2 Sb1 105.03(3) 2_655 . ?
Sb1 K2 Sb1 124.35(3) 2_655 . ?
F2 K2 K1 93.53(6) 2_655 2_655 ?
F1 K2 K1 46.00(5) 2_655 2_655 ?
Cl3 K2 K1 117.66(4) 3_746 2_655 ?
Cl1 K2 K1 136.90(4) 3_756 2_655 ?
Cl2 K2 K1 119.88(4) 4_556 2_655 ?
Cl3 K2 K1 63.72(3) . 2_655 ?
Cl1 K2 K1 52.58(3) . 2_655 ?
Cl2 K2 K1 51.47(3) 2_655 2_655 ?
Sb1 K2 K1 64.16(2) 2_655 2_655 ?
Sb1 K2 K1 61.31(2) . 2_655 ?
F2 K2 K2 120.51(6) 2_655 3_756 ?
F1 K2 K2 102.23(6) 2_655 3_756 ?
Cl3 K2 K2 126.20(5) 3_746 3_756 ?
Cl1 K2 K2 48.06(3) 3_756 3_756 ?
Cl2 K2 K2 53.26(3) 4_556 3_756 ?
Cl3 K2 K2 45.92(3) . 3_756 ?
Cl1 K2 K2 105.71(4) . 3_756 ?
Cl2 K2 K2 157.90(5) 2_655 3_756 ?
Sb1 K2 K2 124.49(3) 2_655 3_756 ?
Sb1 K2 K2 67.46(3) . 3_756 ?
K1 K2 K2 109.63(4) 2_655 3_756 ?
F2 Sb1 F1 83.28(10) . . ?
F2 Sb1 Cl2 83.07(7) . . ?
F1 Sb1 Cl2 83.50(7) . . ?
F2 Sb1 Cl1 80.51(7) . . ?
F1 Sb1 Cl1 84.24(7) . . ?
Cl2 Sb1 Cl1 160.53(4) . . ?
F2 Sb1 Cl3 75.20(7) . . ?
F1 Sb1 Cl3 158.45(8) . . ?
Cl2 Sb1 Cl3 92.61(4) . . ?
Cl1 Sb1 Cl3 93.25(4) . . ?
F2 Sb1 K2 41.73(7) . 2_654 ?
F1 Sb1 K2 47.29(8) . 2_654 ?
Cl2 Sb1 K2 63.64(3) . 2_654 ?
Cl1 Sb1 K2 96.99(3) . 2_654 ?
Cl3 Sb1 K2 112.24(3) . 2_654 ?
F2 Sb1 K2 91.17(7) . . ?
F1 Sb1 K2 133.92(7) . . ?
Cl2 Sb1 K2 141.33(3) . . ?
Cl1 Sb1 K2 49.81(3) . . ?
Cl3 Sb1 K2 49.23(3) . . ?
K2 Sb1 K2 130.055(15) 2_654 . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.38
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.491
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.115
