# Supplementary Material (ESI) for ChemComm
# This journal is © The Royal Society of Chemistry 2000
# CCDC Number: 182/1764


data_MoSb2Se

_audit_creation_method            SHELXL
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_formula_moiety          ?
_chemical_formula_structural      ?
_chemical_formula_analytical      ?
_chemical_formula_sum             'Mo Sb2 Se'
_chemical_formula_weight          418.40
_chemical_melting_point           ?
_chemical_compound_source         ?

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'Se'  'Se'  -0.0929   2.2259
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'Mo'  'Mo'  -1.6832   0.6857
 '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            1
_symmetry_space_group_name_H-M    P21/c

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

_cell_length_a                    6.5728(4)
_cell_length_b                    6.4941(3)
_cell_length_c                    18.2990(10)
_cell_angle_alpha                 90.00
_cell_angle_beta                  94.246(8)
_cell_angle_gamma                 90.00
_cell_volume                      778.94(7)
_cell_formula_units_Z             8
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?

_exptl_crystal_description        needle
_exptl_crystal_colour             black
_exptl_crystal_size_max           0.09
_exptl_crystal_size_mid           0.03
_exptl_crystal_size_min           0.02
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     7.136
_exptl_crystal_density_method     ?
_exptl_crystal_F_000              1424
_exptl_absorpt_coefficient_mu     26.035
_exptl_absorpt_correction_type    numerical
_exptl_absorpt_correction_T_min   0.25
_exptl_absorpt_correction_T_max   0.38

_exptl_special_details
;
 ?
;

_diffrn_ambient_temperature       293(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        ?
_diffrn_measurement_method        ?
_diffrn_standards_number          ?
_diffrn_standards_interval_count  ?
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             13328
_diffrn_reflns_av_R_equivalents   0.0338
_diffrn_reflns_av_sigmaI/netI     0.0199
_diffrn_reflns_limit_h_min        -9
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -8
_diffrn_reflns_limit_k_max        8
_diffrn_reflns_limit_l_min        -25
_diffrn_reflns_limit_l_max        25
_diffrn_reflns_theta_min          3.11
_diffrn_reflns_theta_max          30.27
_reflns_number_total              2214
_reflns_number_observed           1403
_reflns_observed_criterion        2sigma(I)

_computing_data_collection        ?
_computing_cell_refinement        ?
_computing_data_reduction         ?
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics     ?
_computing_publication_material   ?

_refine_special_details
;
 Refinement on F^2^ for ALL reflections except for 0 with very negative 
F^2^
 or flagged by the user for potential systematic errors.  Weighted R-
factors
 wR and all goodnesses 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 observed 
criterion
 of F^2^  2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0200P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     ?
_refine_ls_extinction_method      SHELXL
_refine_ls_extinction_coef        0.00029(5)
_refine_ls_extinction_expression
 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^'
_refine_ls_number_reflns          2214
_refine_ls_number_parameters      74
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0384
_refine_ls_R_factor_obs           0.0205
_refine_ls_wR_factor_all          0.0468
_refine_ls_wR_factor_obs          0.0437
_refine_ls_goodness_of_fit_all    1.038
_refine_ls_goodness_of_fit_obs    1.229
_refine_ls_restrained_S_all       1.038
_refine_ls_restrained_S_obs       1.229
_refine_ls_shift/esd_max          0.193
_refine_ls_shift/esd_mean         0.031

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_thermal_displace_type
 _atom_site_occupancy
 _atom_site_calc_flag
 _atom_site_refinement_flags
 _atom_site_disorder_group
Sb1 Sb 0.07475(3) 0.3744(3) 0.075975(13) 0.00471(7) Uani 1 d . .
Sb2 Sb 0.07472(3) -0.1253(3) 0.075820(13) 0.00484(7) Uani 1 d . .
Sb3 Sb 0.20296(7) 0.3499(2) 0.22816(3) 0.0119(2) Uani 1 d . .
Sb4 Sb 0.20267(7) -0.1001(2) 0.22806(3) 0.0122(2) Uani 1 d . .
Mo1 Mo 0.32480(4) 0.1251(3) -0.00586(2) 0.00324(8) Uani 1 d . .
Mo2 Mo -0.32494(4) 0.3753(3) 0.00574(2) 0.00317(8) Uani 1 d . .
Se1 Se 0.58605(5) 0.1249(4) 0.10200(2) 0.00530(8) Uani 1 d . .
Se2 Se 0.41440(5) 0.3753(4) -0.10202(2) 0.00532(8) Uani 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
Sb1 0.00237(12) 0.00669(14) 0.00528(12) -0.0003(6) 0.00168(8) -0.0008(5)
Sb2 0.00237(12) 0.00685(14) 0.00551(12) -0.0006(6) 0.00166(8) -0.0008(5)
Sb3 0.01436(14) 0.0138(5) 0.00769(13) -0.0004(2) 0.00065(9) -0.0010(2)
Sb4 0.01420(14) 0.0146(5) 0.00782(13) 0.0009(2) 0.00069(9) 0.0009(2)
Mo1 0.00119(14) 0.0043(2) 0.00439(15) 0.0006(7) 0.00107(10) -0.0010(6)
Mo2 0.00114(14) 0.0042(2) 0.00428(15) 0.0007(7) 0.00094(10) -0.0011(6)
Se1 0.0054(2) 0.0057(2) 0.0050(2) 0.0007(9) 0.00110(12) -0.0008(8)
Se2 0.0054(2) 0.0058(2) 0.0048(2) 0.0008(9) 0.00069(12) -0.0007(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
Sb1 Mo1 2.816(2) . ?
Sb1 Mo2 2.819(2) 3_565 ?
Sb1 Mo2 2.8379(4) . ?
Sb1 Sb3 2.8536(6) . ?
Sb1 Sb2 3.2451(3) . ?
Sb1 Sb2 3.2490(3) 1_565 ?
Sb1 Sb2 3.300(2) 3 ?
Sb1 Sb1 3.310(2) 3_565 ?
Sb2 Mo2 2.816(2) 3 ?
Sb2 Mo1 2.819(2) . ?
Sb2 Mo1 2.8349(4) 3 ?
Sb2 Sb4 2.8545(6) . ?
Sb2 Sb1 3.2490(3) 1_545 ?
Sb2 Sb1 3.300(2) 3 ?
Sb2 Sb2 3.303(2) 3 ?
Sb3 Sb4 2.8587(4) 2 ?
Sb3 Sb4 2.9224(4) . ?
Sb4 Sb3 2.8587(4) 2_545 ?
Mo1 Se1 2.495(2) 3_655 ?
Mo1 Se2 2.497(2) . ?
Mo1 Se1 2.5185(5) . ?
Mo1 Mo1 2.814(3) 3_655 ?
Mo1 Mo2 2.813(3) 1_655 ?
Mo1 Sb2 2.8349(4) 3 ?
Mo2 Se2 2.495(2) 3_565 ?
Mo2 Se1 2.498(2) 1_455 ?
Mo2 Se2 2.5146(5) 1_455 ?
Mo2 Mo2 2.809(3) 3_465 ?
Mo2 Mo1 2.813(3) 1_455 ?
Mo2 Sb2 2.816(2) 3 ?
Mo2 Sb1 2.819(2) 3_565 ?
Se1 Mo1 2.495(2) 3_655 ?
Se1 Mo2 2.498(2) 1_655 ?
Se2 Mo2 2.495(2) 3_565 ?
Se2 Mo2 2.5146(5) 1_655 ?

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
Mo1 Sb1 Mo2 70.306(11) . 3_565 ?
Mo1 Sb1 Mo2 108.51(4) . . ?
Mo2 Sb1 Mo2 108.39(4) 3_565 . ?
Mo1 Sb1 Sb3 110.19(4) . . ?
Mo2 Sb1 Sb3 114.08(4) 3_565 . ?
Mo2 Sb1 Sb3 129.69(2) . . ?
Mo1 Sb1 Sb2 54.88(5) . . ?
Mo2 Sb1 Sb2 125.18(5) 3_565 . ?
Mo2 Sb1 Sb2 90.09(6) . . ?
Sb3 Sb1 Sb2 86.86(5) . . ?
Mo1 Sb1 Sb2 125.06(5) . 1_565 ?
Mo2 Sb1 Sb2 54.75(5) 3_565 1_565 ?
Mo2 Sb1 Sb2 89.86(6) . 1_565 ?
Sb3 Sb1 Sb2 93.24(5) . 1_565 ?
Sb2 Sb1 Sb2 179.900(13) . 1_565 ?
Mo1 Sb1 Sb2 54.53(3) . 3 ?
Mo2 Sb1 Sb2 89.15(3) 3_565 3 ?
Mo2 Sb1 Sb2 53.98(3) . 3 ?
Sb3 Sb1 Sb2 147.35(10) . 3 ?
Sb2 Sb1 Sb2 60.60(6) . 3 ?
Sb2 Sb1 Sb2 119.30(6) 1_565 3 ?
Mo1 Sb1 Sb1 89.15(3) . 3_565 ?
Mo2 Sb1 Sb1 54.46(3) 3_565 3_565 ?
Mo2 Sb1 Sb1 53.93(3) . 3_565 ?
Sb3 Sb1 Sb1 153.53(10) . 3_565 ?
Sb2 Sb1 Sb1 119.49(6) . 3_565 ?
Sb2 Sb1 Sb1 60.42(6) 1_565 3_565 ?
Sb2 Sb1 Sb1 58.881(9) 3 3_565 ?
Mo2 Sb2 Mo1 70.440(11) 3 . ?
Mo2 Sb2 Mo1 108.58(4) 3 3 ?
Mo1 Sb2 Mo1 108.50(4) . 3 ?
Mo2 Sb2 Sb4 114.13(4) 3 . ?
Mo1 Sb2 Sb4 110.07(4) . . ?
Mo1 Sb2 Sb4 129.55(2) 3 . ?
Mo2 Sb2 Sb1 125.23(5) 3 . ?
Mo1 Sb2 Sb1 54.79(5) . . ?
Mo1 Sb2 Sb1 90.00(6) 3 . ?
Sb4 Sb2 Sb1 86.66(5) . . ?
Mo2 Sb2 Sb1 54.83(5) 3 1_545 ?
Mo1 Sb2 Sb1 125.27(5) . 1_545 ?
Mo1 Sb2 Sb1 90.04(6) 3 1_545 ?
Sb4 Sb2 Sb1 93.24(5) . 1_545 ?
Sb1 Sb2 Sb1 179.900(9) . 1_545 ?
Mo2 Sb2 Sb1 54.59(3) 3 3 ?
Mo1 Sb2 Sb1 89.17(3) . 3 ?
Mo1 Sb2 Sb1 53.99(3) 3 3 ?
Sb4 Sb2 Sb1 153.81(10) . 3 ?
Sb1 Sb2 Sb1 119.40(6) . 3 ?
Sb1 Sb2 Sb1 60.70(6) 1_545 3 ?
Mo2 Sb2 Sb2 89.30(3) 3 3 ?
Mo1 Sb2 Sb2 54.48(3) . 3 ?
Mo1 Sb2 Sb2 54.02(3) 3 3 ?
Sb4 Sb2 Sb2 147.08(10) . 3 ?
Sb1 Sb2 Sb2 60.53(6) . 3 ?
Sb1 Sb2 Sb2 119.57(6) 1_545 3 ?
Sb1 Sb2 Sb2 58.868(9) 3 3 ?
Sb1 Sb3 Sb4 93.04(2) . 2 ?
Sb1 Sb3 Sb4 93.15(5) . . ?
Sb4 Sb3 Sb4 96.50(2) 2 . ?
Sb2 Sb4 Sb3 93.07(2) . 2_545 ?
Sb2 Sb4 Sb3 93.33(5) . . ?
Sb3 Sb4 Sb3 96.55(2) 2_545 . ?
Se1 Mo1 Se2 81.177(15) 3_655 . ?
Se1 Mo1 Se1 111.71(6) 3_655 . ?
Se2 Mo1 Se1 111.72(6) . . ?
Se1 Mo1 Mo1 56.25(5) 3_655 3_655 ?
Se2 Mo1 Mo1 101.25(4) . 3_655 ?
Se1 Mo1 Mo1 55.47(5) . 3_655 ?
Se1 Mo1 Mo2 101.27(4) 3_655 1_655 ?
Se2 Mo1 Mo2 56.16(5) . 1_655 ?
Se1 Mo1 Mo2 55.56(5) . 1_655 ?
Mo1 Mo1 Mo2 70.557(12) 3_655 1_655 ?
Se1 Mo1 Sb1 157.78(3) 3_655 . ?
Se2 Mo1 Sb1 100.26(9) . . ?
Se1 Mo1 Sb1 88.54(5) . . ?
Mo1 Mo1 Sb1 142.95(2) 3_655 . ?
Mo2 Mo1 Sb1 97.73(10) 1_655 . ?
Se1 Mo1 Sb2 100.08(9) 3_655 . ?
Se2 Mo1 Sb2 157.86(3) . . ?
Se1 Mo1 Sb2 88.54(5) . . ?
Mo1 Mo1 Sb2 97.61(9) 3_655 . ?
Mo2 Mo1 Sb2 143.07(2) 1_655 . ?
Sb1 Mo1 Sb2 70.330(10) . . ?
Se1 Mo1 Sb2 86.55(4) 3_655 3 ?
Se2 Mo1 Sb2 86.59(4) . 3 ?
Se1 Mo1 Sb2 155.36(2) . 3 ?
Mo1 Mo1 Sb2 139.48(10) 3_655 3 ?
Mo2 Mo1 Sb2 139.42(10) 1_655 3 ?
Sb1 Mo1 Sb2 71.48(4) . 3 ?
Sb2 Mo1 Sb2 71.50(4) . 3 ?
Se2 Mo2 Se1 81.082(15) 3_565 1_455 ?
Se2 Mo2 Se2 111.79(6) 3_565 1_455 ?
Se1 Mo2 Se2 111.80(6) 1_455 1_455 ?
Se2 Mo2 Mo2 56.22(5) 3_565 3_465 ?
Se1 Mo2 Mo2 101.23(4) 1_455 3_465 ?
Se2 Mo2 Mo2 55.57(5) 1_455 3_465 ?
Se2 Mo2 Mo1 101.18(4) 3_565 1_455 ?
Se1 Mo2 Mo1 56.24(5) 1_455 1_455 ?
Se2 Mo2 Mo1 55.57(5) 1_455 1_455 ?
Mo2 Mo2 Mo1 70.489(12) 3_465 1_455 ?
Se2 Mo2 Sb2 157.78(3) 3_565 3 ?
Se1 Mo2 Sb2 100.07(9) 1_455 3 ?
Se2 Mo2 Sb2 88.58(5) 1_455 3 ?
Mo2 Mo2 Sb2 143.13(2) 3_465 3 ?
Mo1 Mo2 Sb2 97.70(10) 1_455 3 ?
Se2 Mo2 Sb1 100.22(9) 3_565 3_565 ?
Se1 Mo2 Sb1 157.75(3) 1_455 3_565 ?
Se2 Mo2 Sb1 88.53(5) 1_455 3_565 ?
Mo2 Mo2 Sb1 97.73(9) 3_465 3_565 ?
Mo1 Mo2 Sb1 143.07(2) 1_455 3_565 ?
Sb2 Mo2 Sb1 70.416(10) 3 3_565 ?
Se2 Mo2 Sb1 86.57(4) 3_565 . ?
Se1 Mo2 Sb1 86.37(4) 1_455 . ?
Se2 Mo2 Sb1 155.40(2) 1_455 . ?
Mo2 Mo2 Sb1 139.53(10) 3_465 . ?
Mo1 Mo2 Sb1 139.30(10) 1_455 . ?
Sb2 Mo2 Sb1 71.43(4) 3 . ?
Sb1 Mo2 Sb1 71.61(4) 3_565 . ?
Mo1 Se1 Mo2 81.200(15) 3_655 1_655 ?
Mo1 Se1 Mo1 68.29(6) 3_655 . ?
Mo2 Se1 Mo1 68.20(6) 1_655 . ?
Mo2 Se2 Mo1 81.058(15) 3_565 . ?
Mo2 Se2 Mo2 68.21(6) 3_565 1_655 ?
Mo1 Se2 Mo2 68.28(6) . 1_655 ?

_refine_diff_density_max    1.276
_refine_diff_density_min   -1.459
_refine_diff_density_rms    0.267