 
data_s92 
 
_audit_creation_method            SHELXL 
_chemical_name_systematic 
; 
 ? 
; 
_chemical_name_common             ? 
_chemical_formula_moiety          ? 
_chemical_formula_structural      ? 
_chemical_formula_analytical      ? 
_chemical_formula_sum             'C31 H22 Cl2 I3 Mo N O3 P' 
_chemical_formula_weight          1035.01 
_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 
 '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' 
 'O'  'O'   0.0106   0.0060 
 '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' 
 'P'  'P'   0.1023   0.0942 
 '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' 
 'Cl'  'Cl'   0.1484   0.1585 
 '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' 
 
_symmetry_cell_setting            Triclinic 
_symmetry_space_group_name_H-M    P-1
 
loop_ 
 _symmetry_equiv_pos_as_xyz 
 'x, y, z' 
 '-x, -y, -z' 
 
_cell_length_a                    10.539(21) 
_cell_length_b                    11.209(24) 
_cell_length_c                    16.580(4) 
_cell_angle_alpha                 74.90(5) 
_cell_angle_beta                  77.50(7) 
_cell_angle_gamma                 72.15(5) 
_cell_volume                      1780.0(53) 
_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        ? 
_exptl_crystal_colour             ? 
_exptl_crystal_size_max           0.24 
_exptl_crystal_size_mid           0.14
_exptl_crystal_size_min           0.14
_exptl_crystal_density_meas       ? 
_exptl_crystal_density_diffrn     1.931 
_exptl_crystal_density_method     ? 
_exptl_crystal_F_000              978 
_exptl_absorpt_coefficient_mu     3.196 
_exptl_absorpt_correction_type    ? 
_exptl_absorpt_correction_T_min   ? 
_exptl_absorpt_correction_T_max   ? 
 
_exptl_special_details 
; 
 ? 
; 
 
_diffrn_ambient_temperature       293(2) 
_diffrn_radiation_wavelength      0.71069 
_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             5101 
_diffrn_reflns_av_R_equivalents   0.0532 
_diffrn_reflns_av_sigmaI/netI     0.1204 
_diffrn_reflns_limit_h_min        -10 
_diffrn_reflns_limit_h_max        10 
_diffrn_reflns_limit_k_min        -12 
_diffrn_reflns_limit_k_max        11 
_diffrn_reflns_limit_l_min        -19 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          1.95 
_diffrn_reflns_theta_max          24.72 
_reflns_number_total              3518 
_reflns_number_observed           2345 
_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-92 (Sheldrick, 1993)' 
_computing_molecular_graphics     ? 
_computing_publication_material   ? 
 
_refine_special_details 
; 
 Refinement on F² for ALL reflections except for 3 with very negative F² 
 or flagged by the user for potential systematic errors.  Weighted R-factors 
 wR and all goodnesses of fit S are based on F², conventional R-factors R 
 are based on F, with F set to zero for negative F². The observed criterion 
 of F² > 2sigma(F²) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0744P)^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      none 
_refine_ls_extinction_coef        ? 
_refine_ls_number_reflns          3515 
_refine_ls_number_parameters      379 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0804 
_refine_ls_R_factor_obs           0.0562 
_refine_ls_wR_factor_all          0.1445 
_refine_ls_wR_factor_obs          0.1324 
_refine_ls_goodness_of_fit_all    0.930 
_refine_ls_goodness_of_fit_obs    1.111 
_refine_ls_restrained_S_all       0.964 
_refine_ls_restrained_S_obs       1.111 
_refine_ls_shift/esd_max          0.001 
_refine_ls_shift/esd_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_thermal_displace_type 
 _atom_site_occupancy 
 _atom_site_calc_flag 
 _atom_site_refinement_flags 
 _atom_site_disorder_group 
Mo1 Mo -0.16260(13) 1.05634(10) 0.22852(7) 0.0332(4) Uani 1 d . . 
Cl1 Cl -0.6680(7) 0.9151(6) 0.3594(4) 0.110(3) Uani 1 d . . 
Cl2 Cl -0.5351(6) 0.7013(6) 0.4810(4) 0.119(3) Uani 1 d . . 
I1 I 0.10994(11) 0.90570(9) 0.18616(6) 0.0477(4) Uani 1 d . . 
I2 I -0.23670(12) 0.81740(9) 0.29141(7) 0.0584(4) Uani 1 d . . 
I3 I -0.09729(12) 1.04922(11) 0.39165(6) 0.0599(5) Uani 1 d . . 
P1 P -0.2974(4) 1.2481(3) 0.1390(2) 0.0344(11) Uani 1 d . . 
N1 N 0.0939(17) 0.6726(14) 0.3866(10) 0.070(6) Uani 1 d . . 
O1 O -0.1760(13) 0.9701(9) 0.0644(7) 0.067(4) Uani 1 d . . 
O2 O 0.0129(14) 1.2516(11) 0.1899(8) 0.070(4) Uani 1 d . . 
O3 O -0.4412(13) 1.1320(10) 0.3442(7) 0.069(4) Uani 1 d . . 
C1 C -0.1733(16) 0.9996(13) 0.1227(9) 0.038(4) Uani 1 d . . 
C2 C -0.0531(20) 1.1858(14) 0.2022(11) 0.052(6) Uani 1 d . . 
C3 C -0.3350(17) 1.1086(12) 0.2994(9) 0.041(5) Uani 1 d . . 
C4 C -0.4228(15) 1.2142(12) 0.0931(8) 0.039(5) Uani 1 d . . 
C5 C -0.5163(23) 1.1537(16) 0.1432(13) 0.068(6) Uani 1 d . . 
H5 H -0.5188(23) 1.1350(16) 0.2015(13) 0.082 Uiso 1 calc R . 
C6 C -0.6038(23) 1.1207(19) 0.1115(16) 0.084(8) Uani 1 d . . 
H6 H -0.6649(23) 1.0800(19) 0.1487(16) 0.101 Uiso 1 calc R . 
C7 C -0.6074(21) 1.1446(18) 0.0257(17) 0.083(7) Uani 1 d . . 
H7 H -0.6690(21) 1.1217(18) 0.0041(17) 0.099 Uiso 1 calc R . 
C8 C -0.5109(30) 1.2062(18) -0.0271(14) 0.096(10) Uani 1 d . . 
H8 H -0.5092(30) 1.2255(18) -0.0853(14) 0.115 Uiso 1 calc R . 
C9 C -0.4169(21) 1.2391(15) 0.0070(10) 0.055(5) Uani 1 d . . 
H9 H -0.3522(21) 1.2771(15) -0.0284(10) 0.066 Uiso 1 calc R . 
C10 C -0.1984(15) 1.3311(11) 0.0475(8) 0.030(4) Uani 1 d . . 
C11 C -0.2400(15) 1.4608(13) 0.0170(9) 0.040(5) Uani 1 d . . 
H11 H -0.3200(15) 1.5079(13) 0.0431(9) 0.048 Uiso 1 calc R . 
C12 C -0.1673(20) 1.5230(15) -0.0506(11) 0.074(7) Uani 1 d . . 
H12 H -0.1975(20) 1.6111(15) -0.0697(11) 0.089 Uiso 1 calc R . 
C13 C -0.0476(19) 1.4531(14) -0.0902(10) 0.064(7) Uani 1 d . . 
H13 H 0.0018(19) 1.4947(14) -0.1364(10) 0.077 Uiso 1 calc R . 
C14 C -0.0030(17) 1.3257(12) -0.0622(10) 0.048(5) Uani 1 d . . 
H14 H 0.0771(17) 1.2790(12) -0.0884(10) 0.058 Uiso 1 calc R . 
C15 C -0.0814(18) 1.2633(13) 0.0087(8) 0.056(6) Uani 1 d . . 
H15 H -0.0517(18) 1.1753(13) 0.0284(8) 0.067 Uiso 1 calc R . 
C16 C -0.3981(16) 1.3789(13) 0.1908(9) 0.039(5) Uani 1 d . . 
C17 C -0.3436(20) 1.4136(14) 0.2478(11) 0.063(6) Uani 1 d . . 
H17 H -0.2592(20) 1.3650(14) 0.2615(11) 0.076 Uiso 1 calc R . 
C18 C -0.4120(25) 1.5199(17) 0.2855(11) 0.085(8) Uani 1 d . . 
H18 H -0.3751(25) 1.5421(17) 0.3238(11) 0.101 Uiso 1 calc R . 
C19 C -0.5339(26) 1.5878(19) 0.2629(13) 0.090(10) Uani 1 d . . 
H19 H -0.5814(26) 1.6583(19) 0.2868(13) 0.109 Uiso 1 calc R . 
C20 C -0.5912(21) 1.5575(15) 0.2063(12) 0.073(8) Uani 1 d . . 
H20 H -0.6743(21) 1.6074(15) 0.1912(12) 0.088 Uiso 1 calc R . 
C21 C -0.5209(17) 1.4499(14) 0.1723(9) 0.050(5) Uani 1 d . . 
H21 H -0.5601(17) 1.4265(14) 0.1357(9) 0.059 Uiso 1 calc R . 
C22 C 0.1119(21) 0.7033(18) 0.4548(14) 0.072(7) Uani 1 d . . 
H22 H 0.0911(21) 0.7891(18) 0.4576(14) 0.086 Uiso 1 calc R . 
C23 C 0.1574(22) 0.6162(16) 0.5167(13) 0.075(7) Uani 1 d . . 
H23 H 0.1648(22) 0.6423(16) 0.5639(13) 0.090 Uiso 1 calc R . 
C24 C 0.1947(20) 0.4914(17) 0.5182(12) 0.066(6) Uani 1 d . . 
H24 H 0.2303(20) 0.4330(17) 0.5642(12) 0.079 Uiso 1 calc R . 
C25 C 0.1799(22) 0.4499(14) 0.4510(11) 0.068(7) Uani 1 d . . 
C26 C 0.2084(23) 0.3144(17) 0.4422(16) 0.078(8) Uani 1 d . . 
H26 H 0.2405(23) 0.2475(17) 0.4857(16) 0.093 Uiso 1 calc R . 
C27 C 0.1889(28) 0.2890(23) 0.3746(17) 0.109(11) Uani 1 d . . 
H27 H 0.2074(28) 0.2041(23) 0.3702(17) 0.131 Uiso 1 calc R . 
C28 C 0.1406(27) 0.3868(27) 0.3085(20) 0.117(10) Uani 1 d . . 
H28 H 0.1306(27) 0.3646(27) 0.2604(20) 0.140 Uiso 1 calc R . 
C29 C 0.1076(24) 0.5122(22) 0.3107(13) 0.083(8) Uani 1 d . . 
H29 H 0.0764(24) 0.5760(22) 0.2655(13) 0.100 Uiso 1 calc R . 
C30 C 0.1226(18) 0.5404(20) 0.3826(11) 0.060(6) Uani 1 d . . 
C31 C -0.5737(22) 0.8698(19) 0.4536(14) 0.097(9) Uani 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 
Mo1 C3 1.95(2) . ? 
Mo1 C2 2.03(2) . ? 
Mo1 C1 2.05(2) . ? 
Mo1 P1 2.494(5) . ? 
Mo1 I2 2.889(6) . ? 
Mo1 I1 2.892(5) . ? 
Mo1 I3 2.908(2) . ? 
Cl1 C31 1.91(3) . ? 
Cl2 C31 1.76(2) . ? 
P1 C16 1.822(14) . ? 
P1 C4 1.83(2) . ? 
P1 C10 1.852(14) . ? 
N1 C22 1.33(3) . ? 
N1 C30 1.43(3) . ? 
O1 C1 1.11(2) . ? 
O2 C2 1.11(2) . ? 
O3 C3 1.20(2) . ? 
C4 C9 1.37(2) . ? 
C4 C5 1.37(2) . ? 
C5 C6 1.34(3) . ? 
C6 C7 1.38(3) . ? 
C7 C8 1.42(3) . ? 
C8 C9 1.42(3) . ? 
C10 C15 1.36(2) . ? 
C10 C11 1.37(2) . ? 
C11 C12 1.37(2) . ? 
C12 C13 1.39(2) . ? 
C13 C14 1.35(2) . ? 
C14 C15 1.43(2) . ? 
C16 C21 1.35(2) . ? 
C16 C17 1.39(3) . ? 
C17 C18 1.41(2) . ? 
C18 C19 1.35(3) . ? 
C19 C20 1.38(3) . ? 
C20 C21 1.40(2) . ? 
C22 C23 1.28(2) . ? 
C23 C24 1.33(2) . ? 
C24 C25 1.37(3) . ? 
C25 C30 1.41(2) . ? 
C25 C26 1.49(3) . ? 
C26 C27 1.30(3) . ? 
C27 C28 1.39(3) . ? 
C28 C29 1.35(3) . ? 
C29 C30 1.36(3) . ? 
 
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 
C3 Mo1 C2 112.6(6) . . ? 
C3 Mo1 C1 115.1(7) . . ? 
C2 Mo1 C1 112.4(7) . . ? 
C3 Mo1 P1 74.5(4) . . ? 
C2 Mo1 P1 76.1(5) . . ? 
C1 Mo1 P1 73.7(4) . . ? 
C3 Mo1 I2 78.2(4) . . ? 
C2 Mo1 I2 160.1(5) . . ? 
C1 Mo1 I2 75.0(4) . . ? 
P1 Mo1 I2 123.7(2) . . ? 
C3 Mo1 I1 157.0(4) . . ? 
C2 Mo1 I1 76.9(5) . . ? 
C1 Mo1 I1 77.4(4) . . ? 
P1 Mo1 I1 128.46(11) . . ? 
I2 Mo1 I1 87.32(14) . . ? 
C3 Mo1 I3 74.2(5) . . ? 
C2 Mo1 I3 76.1(5) . . ? 
C1 Mo1 I3 161.1(3) . . ? 
P1 Mo1 I3 125.23(13) . . ? 
I2 Mo1 I3 91.77(8) . . ? 
I1 Mo1 I3 88.72(11) . . ? 
C16 P1 C4 102.5(8) . . ? 
C16 P1 C10 102.1(6) . . ? 
C4 P1 C10 104.5(7) . . ? 
C16 P1 Mo1 116.6(5) . . ? 
C4 P1 Mo1 114.1(4) . . ? 
C10 P1 Mo1 115.3(5) . . ? 
C22 N1 C30 119.9(15) . . ? 
O1 C1 Mo1 178.0(16) . . ? 
O2 C2 Mo1 176.0(17) . . ? 
O3 C3 Mo1 175.4(12) . . ? 
C9 C4 C5 118.8(19) . . ? 
C9 C4 P1 120.1(14) . . ? 
C5 C4 P1 120.9(14) . . ? 
C6 C5 C4 122.5(20) . . ? 
C5 C6 C7 122.8(22) . . ? 
C6 C7 C8 115.5(25) . . ? 
C7 C8 C9 121.4(21) . . ? 
C4 C9 C8 119.0(18) . . ? 
C15 C10 C11 118.3(12) . . ? 
C15 C10 P1 120.0(9) . . ? 
C11 C10 P1 121.7(10) . . ? 
C12 C11 C10 122.1(13) . . ? 
C11 C12 C13 119.4(13) . . ? 
C14 C13 C12 120.4(13) . . ? 
C13 C14 C15 118.9(13) . . ? 
C10 C15 C14 120.9(12) . . ? 
C21 C16 C17 117.9(15) . . ? 
C21 C16 P1 122.7(16) . . ? 
C17 C16 P1 119.3(12) . . ? 
C16 C17 C18 122.3(18) . . ? 
C19 C18 C17 116.5(24) . . ? 
C18 C19 C20 123.2(19) . . ? 
C19 C20 C21 118.1(18) . . ? 
C16 C21 C20 122.0(21) . . ? 
C23 C22 N1 120.9(20) . . ? 
C22 C23 C24 124.6(24) . . ? 
C23 C24 C25 119.0(17) . . ? 
C24 C25 C30 119.4(17) . . ? 
C24 C25 C26 127.4(18) . . ? 
C30 C25 C26 113.0(21) . . ? 
C27 C26 C25 120.7(21) . . ? 
C26 C27 C28 121.0(26) . . ? 
C29 C28 C27 123.3(30) . . ? 
C28 C29 C30 116.4(22) . . ? 
C29 C30 C25 125.1(20) . . ? 
C29 C30 N1 118.5(17) . . ? 
C25 C30 N1 115.9(19) . . ? 
Cl2 C31 Cl1 104.5(14) . . ? 
 
_refine_diff_density_max    1.875 
_refine_diff_density_min   -0.813 
_refine_diff_density_rms    0.156 
