 
data_solution
 
_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
 ?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          'C23 H18 I2 N O3 Sb W, C H2 Cl2'
_chemical_formula_sum
 'C24 H20 Cl2 I2 N O3 Sb W'
_chemical_formula_weight          1000.71
 
loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0033   0.0016
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'N'  'N'   0.0061   0.0033
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'O'  'O'   0.0106   0.0060
 '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'
 'I'  'I'  -0.4742   1.8119
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'W'  'W'  -0.8490   6.8722
 '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'
 
_symmetry_cell_setting            monoclinic
_symmetry_space_group_name_H-M    P2(1)/c
_symmetry_space_group_name_hall   '-P 2ybc'
 
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                    8.5320(17)
_cell_length_b                    26.226(5)
_cell_length_c                    13.132(3)
_cell_angle_alpha                 90.00
_cell_angle_beta                  96.29(3)
_cell_angle_gamma                 90.00
_cell_volume                      2920.7(10)
_cell_formula_units_Z             4
_cell_measurement_temperature     293(2)
_cell_measurement_reflns_used     ?
_cell_measurement_theta_min       ?
_cell_measurement_theta_max       ?
 
_exptl_crystal_description        unk
_exptl_crystal_colour             unk
_exptl_crystal_size_max           0.2
_exptl_crystal_size_mid           0.2
_exptl_crystal_size_min           0.2
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     2.276
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              1840
_exptl_absorpt_coefficient_mu     7.182
_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       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  'Delft instruments FAST area detector'
_diffrn_measurement_method
 'Intensity measurements as described by Darr, Drake, Hursthouse & Malik (1993)'
_diffrn_standards_number         'None'
_diffrn_standards_interval_count 'N/A'
_diffrn_standards_interval_time  'N/A'
_diffrn_standards_decay_%        'N/A'
_diffrn_reflns_number             8181
_diffrn_reflns_av_R_equivalents   0.0499
_diffrn_reflns_av_sigmaI/netI     0.1511
_diffrn_reflns_limit_h_min        -7
_diffrn_reflns_limit_h_max        9
_diffrn_reflns_limit_k_min        -29
_diffrn_reflns_limit_k_max        16
_diffrn_reflns_limit_l_min        -14
_diffrn_reflns_limit_l_max        14
_diffrn_reflns_theta_min          3.12
_diffrn_reflns_theta_max          24.81
_reflns_number_total              4110
_reflns_number_gt                 3269
_reflns_threshold_expression      >2σ(I)
 
_computing_data_collection        'MADNES (Pflugrath & Messerschmidt, 1989)'
_computing_cell_refinement        REFINE
_computing_data_reduction         'ABSURD (Karaulov, 1992)'
_computing_structure_solution     'SIR92 (Altomare, Cascarano, Giacovazzo & Guaglitardi, 1993)'
_computing_structure_refinement   'SHELXL97 (Sheldrick, 2008)'
_computing_publication_material   SHELXL97
 
_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 > 2σ(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)+(0.0001P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      direct
_atom_sites_solution_secondary    difmap
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          4110
_refine_ls_number_parameters      308
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0449
_refine_ls_R_factor_gt            0.0367
_refine_ls_wR_factor_ref          0.1013
_refine_ls_wR_factor_gt           0.0905
_refine_ls_goodness_of_fit_ref    0.559
_refine_ls_restrained_S_all       0.559
_refine_ls_shift/su_max           0.000
_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
W1 W 0.27568(4) 0.047719(14) 0.32592(3) 0.01777(14) Uani 1 1 d . . .
Sb1 Sb 0.12950(7) 0.13261(2) 0.23197(4) 0.01834(18) Uani 1 1 d . . .
I1 I 0.35025(8) 0.04062(2) 0.11910(5) 0.02442(18) Uani 1 1 d . . .
I2 I 0.37947(8) -0.05591(2) 0.34808(5) 0.02828(19) Uani 1 1 d . . .
N1 N 0.0417(10) 0.0194(3) 0.2687(6) 0.0216(18) Uani 1 1 d . . .
O2 O 0.3414(8) 0.1391(3) 0.4772(5) 0.0340(18) Uani 1 1 d . . .
C21 C 0.2820(11) 0.1866(4) 0.1753(7) 0.021(2) Uani 1 1 d . . .
C8 C -0.0651(13) 0.1595(5) 0.4083(8) 0.039(3) Uani 1 1 d . . .
H8 H -0.0572 0.1247 0.4215 0.047 Uiso 1 1 calc R . .
C20 C 0.2471(12) 0.2090(4) 0.0774(8) 0.031(3) Uani 1 1 d . . .
H20 H 0.1563 0.1993 0.0363 0.037 Uiso 1 1 calc R . .
C22 C -0.0746(13) 0.0053(4) 0.2289(7) 0.026(2) Uani 1 1 d . . .
C15 C -0.0570(12) 0.1230(4) 0.1107(7) 0.023(2) Uani 1 1 d . . .
C16 C 0.4190(12) 0.2019(4) 0.2344(8) 0.030(3) Uani 1 1 d . . .
H16 H 0.4450 0.1876 0.2988 0.036 Uiso 1 1 calc R . .
C10 C -0.2071(12) 0.1371(4) 0.1259(7) 0.027(2) Uani 1 1 d . . .
H10 H -0.2260 0.1510 0.1885 0.033 Uiso 1 1 calc R . .
C9 C 0.0086(11) 0.1814(4) 0.3294(7) 0.023(2) Uani 1 1 d . . .
C18 C 0.4796(13) 0.2605(4) 0.1043(9) 0.037(3) Uani 1 1 d . . .
H18 H 0.5437 0.2861 0.0823 0.044 Uiso 1 1 calc R . .
C5 C -0.0896(13) 0.2639(5) 0.3703(9) 0.038(3) Uani 1 1 d . . .
H5 H -0.0976 0.2987 0.3577 0.045 Uiso 1 1 calc R . .
C23 C -0.2255(13) -0.0118(4) 0.1754(8) 0.037(3) Uani 1 1 d . . .
H23A H -0.2643 0.0134 0.1259 0.055 Uiso 1 1 calc R . .
H23B H -0.3003 -0.0164 0.2241 0.055 Uiso 1 1 calc R . .
H23C H -0.2105 -0.0435 0.1412 0.055 Uiso 1 1 calc R . .
C19 C 0.3468(13) 0.2452(4) 0.0421(9) 0.037(3) Uani 1 1 d . . .
H19 H 0.3244 0.2590 -0.0230 0.045 Uiso 1 1 calc R . .
C4 C -0.0061(13) 0.2332(4) 0.3109(8) 0.033(3) Uani 1 1 d . . .
H4 H 0.0414 0.2475 0.2572 0.039 Uiso 1 1 calc R . .
C2 C 0.3131(12) 0.1058(4) 0.4202(8) 0.028(2) Uani 1 1 d . . .
C12 C -0.3060(12) 0.1102(4) -0.0418(8) 0.030(3) Uani 1 1 d . . .
H12 H -0.3897 0.1052 -0.0924 0.036 Uiso 1 1 calc R . .
C6 C -0.1604(13) 0.2426(5) 0.4480(9) 0.048(4) Uani 1 1 d . . .
H6 H -0.2161 0.2633 0.4890 0.057 Uiso 1 1 calc R . .
C13 C -0.1536(12) 0.0963(4) -0.0603(7) 0.030(3) Uani 1 1 d . . .
H13 H -0.1360 0.0828 -0.1236 0.035 Uiso 1 1 calc R . .
C14 C -0.0272(12) 0.1026(4) 0.0161(7) 0.028(2) Uani 1 1 d . . .
H14 H 0.0746 0.0934 0.0044 0.034 Uiso 1 1 calc R . .
C11 C -0.3328(12) 0.1310(4) 0.0487(7) 0.028(2) Uani 1 1 d . . .
H11 H -0.4339 0.1412 0.0598 0.034 Uiso 1 1 calc R . .
C17 C 0.5174(13) 0.2382(4) 0.1985(9) 0.039(3) Uani 1 1 d . . .
H17 H 0.6097 0.2475 0.2385 0.046 Uiso 1 1 calc R . .
C7 C -0.1510(15) 0.1912(5) 0.4669(9) 0.051(4) Uani 1 1 d . . .
H7 H -0.2025 0.1773 0.5193 0.061 Uiso 1 1 calc R . .
O1 O 0.6424(10) 0.0652(3) 0.3523(6) 0.040(2) Uani 1 1 d . . .
C1 C 0.5074(15) 0.0577(4) 0.3461(8) 0.029(3) Uani 1 1 d . . .
C3 C 0.2097(12) 0.0265(4) 0.4610(8) 0.030(2) Uani 1 1 d . . .
O3 O 0.1687(9) 0.0162(3) 0.5385(6) 0.042(2) Uani 1 1 d . . .
Cl2 Cl -0.0417(4) -0.12002(13) 0.3136(2) 0.0528(8) Uani 1 1 d . . .
Cl1 Cl -0.2935(4) -0.15660(13) 0.1630(2) 0.0541(9) Uani 1 1 d . . .
C50 C -0.2323(15) -0.1464(5) 0.2942(9) 0.052(3) Uani 1 1 d . . .
H50A H -0.3060 -0.1237 0.3224 0.063 Uiso 1 1 calc R . .
H50B H -0.2333 -0.1786 0.3305 0.063 Uiso 1 1 calc R . .
 
 
_geom_special_details
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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
W1 C2 1.966(11) . ?
W1 C1 1.983(13) . ?
W1 C3 1.998(11) . ?
W1 N1 2.184(8) . ?
W1 Sb1 2.7743(8) . ?
W1 I1 2.8627(9) . ?
W1 I2 2.8633(9) . ?
Sb1 C21 2.113(10) . ?
Sb1 C15 2.140(10) . ?
Sb1 C9 2.152(9) . ?
N1 C22 1.132(12) . ?
O2 C2 1.159(12) . ?
C21 C16 1.389(14) . ?
C21 C20 1.414(14) . ?
C8 C9 1.394(14) . ?
C8 C7 1.394(15) . ?
C8 H8 0.9300 . ?
C20 C19 1.388(14) . ?
C20 H20 0.9300 . ?
C22 C23 1.467(15) . ?
C15 C10 1.368(14) . ?
C15 C14 1.401(14) . ?
C16 C17 1.386(15) . ?
C16 H16 0.9300 . ?
C10 C11 1.401(13) . ?
C10 H10 0.9300 . ?
C9 C4 1.383(14) . ?
C18 C17 1.375(15) . ?
C18 C19 1.382(15) . ?
C18 H18 0.9300 . ?
C5 C6 1.362(17) . ?
C5 C4 1.373(14) . ?
C5 H5 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C19 H19 0.9300 . ?
C4 H4 0.9300 . ?
C12 C11 1.350(14) . ?
C12 C13 1.397(14) . ?
C12 H12 0.9300 . ?
C6 C7 1.371(18) . ?
C6 H6 0.9300 . ?
C13 C14 1.400(13) . ?
C13 H13 0.9300 . ?
C14 H14 0.9300 . ?
C11 H11 0.9300 . ?
C17 H17 0.9300 . ?
C7 H7 0.9300 . ?
O1 C1 1.162(12) . ?
C3 O3 1.144(12) . ?
Cl2 C50 1.760(13) . ?
Cl1 C50 1.765(12) . ?
C50 H50A 0.9700 . ?
C50 H50B 0.9700 . ?
 
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
C2 W1 C1 73.9(4) . . ?
C2 W1 C3 72.5(4) . . ?
C1 W1 C3 107.0(4) . . ?
C2 W1 N1 124.0(4) . . ?
C1 W1 N1 162.0(4) . . ?
C3 W1 N1 82.8(4) . . ?
C2 W1 Sb1 72.1(3) . . ?
C1 W1 Sb1 110.3(3) . . ?
C3 W1 Sb1 117.5(3) . . ?
N1 W1 Sb1 76.7(2) . . ?
C2 W1 I1 127.6(3) . . ?
C1 W1 I1 79.2(3) . . ?
C3 W1 I1 159.7(3) . . ?
N1 W1 I1 86.6(2) . . ?
Sb1 W1 I1 76.48(2) . . ?
C2 W1 I2 130.1(3) . . ?
C1 W1 I2 79.6(3) . . ?
C3 W1 I2 76.1(3) . . ?
N1 W1 I2 88.5(2) . . ?
Sb1 W1 I2 157.80(2) . . ?
I1 W1 I2 86.34(2) . . ?
C21 Sb1 C15 104.7(4) . . ?
C21 Sb1 C9 99.5(4) . . ?
C15 Sb1 C9 98.4(4) . . ?
C21 Sb1 W1 115.5(3) . . ?
C15 Sb1 W1 119.9(3) . . ?
C9 Sb1 W1 115.8(3) . . ?
C22 N1 W1 172.6(8) . . ?
C16 C21 C20 117.9(9) . . ?
C16 C21 Sb1 120.6(7) . . ?
C20 C21 Sb1 121.4(7) . . ?
C9 C8 C7 118.1(11) . . ?
C9 C8 H8 121.0 . . ?
C7 C8 H8 121.0 . . ?
C19 C20 C21 120.7(10) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 . . ?
N1 C22 C23 178.5(11) . . ?
C10 C15 C14 119.8(9) . . ?
C10 C15 Sb1 119.4(7) . . ?
C14 C15 Sb1 120.8(7) . . ?
C17 C16 C21 120.8(10) . . ?
C17 C16 H16 119.6 . . ?
C21 C16 H16 119.6 . . ?
C15 C10 C11 121.2(9) . . ?
C15 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C4 C9 C8 119.8(10) . . ?
C4 C9 Sb1 121.3(7) . . ?
C8 C9 Sb1 118.7(8) . . ?
C17 C18 C19 120.2(10) . . ?
C17 C18 H18 119.9 . . ?
C19 C18 H18 119.9 . . ?
C6 C5 C4 119.1(11) . . ?
C6 C5 H5 120.5 . . ?
C4 C5 H5 120.5 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C18 C19 C20 119.7(10) . . ?
C18 C19 H19 120.2 . . ?
C20 C19 H19 120.2 . . ?
C5 C4 C9 121.2(10) . . ?
C5 C4 H4 119.4 . . ?
C9 C4 H4 119.4 . . ?
O2 C2 W1 177.1(9) . . ?
C11 C12 C13 120.6(9) . . ?
C11 C12 H12 119.7 . . ?
C13 C12 H12 119.7 . . ?
C5 C6 C7 121.1(11) . . ?
C5 C6 H6 119.4 . . ?
C7 C6 H6 119.4 . . ?
C12 C13 C14 120.2(9) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C15 118.7(10) . . ?
C13 C14 H14 120.7 . . ?
C15 C14 H14 120.7 . . ?
C12 C11 C10 119.5(10) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C18 C17 C16 120.5(10) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C6 C7 C8 120.7(12) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
O1 C1 W1 175.8(9) . . ?
O3 C3 W1 177.3(9) . . ?
Cl2 C50 Cl1 111.7(7) . . ?
Cl2 C50 H50A 109.3 . . ?
Cl1 C50 H50A 109.3 . . ?
Cl2 C50 H50B 109.3 . . ?
Cl1 C50 H50B 109.3 . . ?
H50A C50 H50B 107.9 . . ?
 
_diffrn_measured_fraction_theta_max    0.817
_diffrn_reflns_theta_full              24.81
_diffrn_measured_fraction_theta_full   0.817
_refine_diff_density_max    1.684
_refine_diff_density_min   -1.671
_refine_diff_density_rms    0.204
