# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Rosa Llusar' _publ_contact_author_email ROSA.LLUSAR@QFA.UJI.ES _publ_section_title ; A Three Dimensional Adamantane-like Nanoscopic Cage Built from Four Iodide-Bridged Triangular Mo3S7 Cluster Units ; loop_ _publ_author_name 'Rosa Llusar' 'Larry Falvello' 'Sonia Triguero' 'Cristian Vicent' # Attachment 'ESI_cif_Chem_Commun_Llusar_revised.txt' data_(PPh4)2[1] _database_code_depnum_ccdc_archive 'CCDC 713962' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 Cl12 Mo3 O6 S7, 2(C24 H20 P), C H2 Cl2' _chemical_formula_sum 'C67 H42 Cl14 Mo3 O6 P2 S7' _chemical_formula_weight 2013.49 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' P P 0.1023 0.0942 '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' 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 Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 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 20.565(4) _cell_length_b 25.840(5) _cell_length_c 14.510(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.27(3) _cell_angle_gamma 90.00 _cell_volume 7610(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 996 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 21.65 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3992 _exptl_absorpt_coefficient_mu 1.263 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.83418 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details 'Bruker SADABS' _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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42587 _diffrn_reflns_av_R_equivalents 0.1044 _diffrn_reflns_av_sigmaI/netI 0.1201 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.00 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13370 _reflns_number_gt 7461 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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 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^)+(0.0896P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13370 _refine_ls_number_parameters 889 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1339 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1857 _refine_ls_wR_factor_gt 0.1492 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 Mo1 Mo 0.21865(4) 0.51045(3) 0.77176(5) 0.0329(2) Uani 1 1 d . . . Mo2 Mo 0.31163(4) 0.58800(3) 0.79338(5) 0.0317(2) Uani 1 1 d . . . Mo3 Mo 0.23526(3) 0.57106(3) 0.93068(5) 0.0305(2) Uani 1 1 d . . . S1 S 0.31395(10) 0.51291(9) 0.88693(15) 0.0331(5) Uani 1 1 d . . . S2 S 0.22174(11) 0.58096(10) 0.66454(16) 0.0421(6) Uani 1 1 d . . . S3 S 0.29294(12) 0.52844(10) 0.65413(16) 0.0434(6) Uani 1 1 d . . . S4 S 0.13389(11) 0.56143(9) 0.82446(16) 0.0400(6) Uani 1 1 d . . . S5 S 0.15507(11) 0.49736(9) 0.90433(17) 0.0410(6) Uani 1 1 d . . . S6 S 0.24225(11) 0.65205(9) 0.85023(16) 0.0400(6) Uani 1 1 d . . . S7 S 0.32505(11) 0.63887(9) 0.94371(17) 0.0418(6) Uani 1 1 d . . . Cl1 Cl 0.27673(15) 0.32155(11) 0.7524(2) 0.0667(8) Uani 1 1 d . . . Cl2 Cl 0.17985(19) 0.26222(12) 0.5974(2) 0.0863(11) Uani 1 1 d . . . Cl3 Cl 0.05853(18) 0.31963(15) 0.4881(2) 0.0985(12) Uani 1 1 d . . . Cl4 Cl 0.03763(15) 0.43787(14) 0.5251(2) 0.0788(10) Uani 1 1 d . . . Cl5 Cl 0.08249(13) 0.65717(10) 1.12741(19) 0.0575(7) Uani 1 1 d . . . Cl6 Cl 0.10770(13) 0.61694(11) 1.33538(18) 0.0597(7) Uani 1 1 d . . . Cl7 Cl 0.22082(15) 0.53812(11) 1.39820(17) 0.0610(7) Uani 1 1 d . . . Cl8 Cl 0.30940(12) 0.49992(10) 1.25298(17) 0.0511(6) Uani 1 1 d . . . Cl9 Cl 0.55495(11) 0.55466(9) 0.82786(18) 0.0494(6) Uani 1 1 d . . . Cl10 Cl 0.63086(12) 0.64148(10) 0.73685(19) 0.0555(7) Uani 1 1 d . . . Cl11 Cl 0.55278(14) 0.73238(10) 0.63055(19) 0.0617(8) Uani 1 1 d . . . Cl12 Cl 0.39896(13) 0.73851(10) 0.62056(19) 0.0567(7) Uani 1 1 d . . . O1 O 0.2418(3) 0.4332(2) 0.7675(4) 0.0428(16) Uani 1 1 d . . . O2 O 0.1422(3) 0.4815(3) 0.6708(4) 0.0453(16) Uani 1 1 d . . . O3 O 0.4114(3) 0.5744(2) 0.8086(4) 0.0364(14) Uani 1 1 d . . . O4 O 0.3445(3) 0.6498(2) 0.7179(4) 0.0407(15) Uani 1 1 d . . . O5 O 0.1749(3) 0.6114(2) 1.0116(4) 0.0407(15) Uani 1 1 d . . . O6 O 0.2686(3) 0.5439(2) 1.0629(4) 0.0371(15) Uani 1 1 d . . . C1 C 0.2015(5) 0.4051(4) 0.7053(6) 0.040(2) Uani 1 1 d . . . C2 C 0.2094(5) 0.3536(4) 0.6876(7) 0.048(3) Uani 1 1 d . . . C3 C 0.1642(7) 0.3268(4) 0.6206(8) 0.065(3) Uani 1 1 d . . . C4 C 0.1106(6) 0.3526(5) 0.5718(9) 0.069(3) Uani 1 1 d . . . C5 C 0.1032(5) 0.4050(5) 0.5879(7) 0.056(3) Uani 1 1 d . . . C6 C 0.1471(5) 0.4323(4) 0.6534(6) 0.045(2) Uani 1 1 d . . . C7 C 0.1841(4) 0.5967(3) 1.1008(6) 0.037(2) Uani 1 1 d . . . C8 C 0.1453(4) 0.6148(3) 1.1642(6) 0.037(2) Uani 1 1 d . . . C9 C 0.1555(4) 0.5960(3) 1.2555(6) 0.038(2) Uani 1 1 d . . . C10 C 0.2057(4) 0.5604(3) 1.2838(6) 0.038(2) Uani 1 1 d . . . C11 C 0.2453(4) 0.5435(3) 1.2208(6) 0.038(2) Uani 1 1 d . . . C12 C 0.2343(4) 0.5596(3) 1.1280(6) 0.035(2) Uani 1 1 d . . . C13 C 0.4090(5) 0.6502(3) 0.7184(6) 0.036(2) Uani 1 1 d . . . C14 C 0.4431(5) 0.6878(3) 0.6770(6) 0.040(2) Uani 1 1 d . . . C15 C 0.5112(5) 0.6851(4) 0.6809(6) 0.041(2) Uani 1 1 d . . . C16 C 0.5462(4) 0.6435(4) 0.7292(7) 0.041(2) Uani 1 1 d . . . C17 C 0.5117(4) 0.6061(3) 0.7706(6) 0.034(2) Uani 1 1 d . . . C18 C 0.4451(4) 0.6091(3) 0.7665(6) 0.035(2) Uani 1 1 d . . . P100 P 0.47865(12) 0.63935(10) 0.33244(17) 0.0402(6) Uani 1 1 d . . . C100 C 0.3963(5) 0.6450(4) 0.3575(7) 0.044(2) Uani 1 1 d . . . C101 C 0.3473(5) 0.6684(4) 0.2948(9) 0.068(3) Uani 1 1 d . . . H101 H 0.3549 0.6768 0.2351 0.082 Uiso 1 1 calc R . . C102 C 0.2873(6) 0.6792(5) 0.3209(11) 0.079(4) Uani 1 1 d . . . H102 H 0.2545 0.6952 0.2789 0.095 Uiso 1 1 calc R . . C103 C 0.2757(7) 0.6667(5) 0.4072(10) 0.081(4) Uani 1 1 d . . . H103 H 0.2349 0.6739 0.4242 0.097 Uiso 1 1 calc R . . C104 C 0.3238(6) 0.6436(5) 0.4695(8) 0.072(4) Uani 1 1 d . . . H104 H 0.3156 0.6353 0.5289 0.086 Uiso 1 1 calc R . . C105 C 0.3843(5) 0.6326(4) 0.4451(7) 0.051(3) Uani 1 1 d . . . H105 H 0.4169 0.6168 0.4877 0.062 Uiso 1 1 calc R . . C106 C 0.4774(5) 0.6210(4) 0.2125(6) 0.041(2) Uani 1 1 d . . . C107 C 0.5330(5) 0.6278(4) 0.1717(7) 0.058(3) Uani 1 1 d . . . H107 H 0.5676 0.6481 0.2007 0.070 Uiso 1 1 calc R . . C108 C 0.5367(7) 0.6040(5) 0.0874(8) 0.077(4) Uani 1 1 d . . . H108 H 0.5745 0.6077 0.0604 0.092 Uiso 1 1 calc R . . C109 C 0.4852(7) 0.5752(5) 0.0433(8) 0.072(4) Uani 1 1 d . . . H109 H 0.4876 0.5602 -0.0143 0.086 Uiso 1 1 calc R . . C110 C 0.4306(6) 0.5682(4) 0.0835(7) 0.058(3) Uani 1 1 d . . . H110 H 0.3962 0.5478 0.0542 0.069 Uiso 1 1 calc R . . C111 C 0.4264(5) 0.5914(4) 0.1675(7) 0.048(3) Uani 1 1 d . . . H111 H 0.3886 0.5870 0.1943 0.057 Uiso 1 1 calc R . . C112 C 0.5200(5) 0.6997(3) 0.3647(6) 0.040(2) Uani 1 1 d . . . C113 C 0.4837(5) 0.7431(4) 0.3864(7) 0.048(3) Uani 1 1 d . . . H113 H 0.4382 0.7414 0.3822 0.058 Uiso 1 1 calc R . . C114 C 0.5172(6) 0.7878(4) 0.4139(7) 0.055(3) Uani 1 1 d . . . H114 H 0.4940 0.8169 0.4278 0.066 Uiso 1 1 calc R . . C115 C 0.5848(7) 0.7901(4) 0.4212(8) 0.067(3) Uani 1 1 d . . . H115 H 0.6066 0.8206 0.4415 0.080 Uiso 1 1 calc R . . C116 C 0.6204(6) 0.7481(5) 0.3990(8) 0.065(3) Uani 1 1 d . . . H116 H 0.6659 0.7503 0.4022 0.078 Uiso 1 1 calc R . . C117 C 0.5880(5) 0.7030(4) 0.3719(7) 0.056(3) Uani 1 1 d . . . H117 H 0.6118 0.6742 0.3582 0.067 Uiso 1 1 calc R . . C118 C 0.5234(4) 0.5884(3) 0.4013(6) 0.038(2) Uani 1 1 d . . . C119 C 0.5572(5) 0.5981(4) 0.4892(6) 0.049(3) Uani 1 1 d . . . H119 H 0.5575 0.6311 0.5148 0.059 Uiso 1 1 calc R . . C120 C 0.5908(5) 0.5578(4) 0.5391(7) 0.050(3) Uani 1 1 d . . . H120 H 0.6116 0.5638 0.5999 0.060 Uiso 1 1 calc R . . C121 C 0.5940(5) 0.5102(4) 0.5024(7) 0.052(3) Uani 1 1 d . . . H121 H 0.6189 0.4844 0.5360 0.062 Uiso 1 1 calc R . . C122 C 0.5599(5) 0.5001(4) 0.4137(7) 0.051(3) Uani 1 1 d . . . H122 H 0.5605 0.4670 0.3890 0.061 Uiso 1 1 calc R . . C123 C 0.5247(4) 0.5393(4) 0.3613(7) 0.042(2) Uani 1 1 d . . . H123 H 0.5026 0.5329 0.3012 0.051 Uiso 1 1 calc R . . P200 P 0.11124(12) 0.37602(10) 0.19942(17) 0.0400(6) Uani 1 1 d . . . C200 C 0.0470(5) 0.3281(4) 0.1882(7) 0.050(3) Uani 1 1 d . . . C201 C -0.0114(5) 0.3383(4) 0.1274(7) 0.051(3) Uani 1 1 d . . . H201 H -0.0167 0.3694 0.0948 0.061 Uiso 1 1 calc R . . C202 C -0.0607(5) 0.3025(5) 0.1161(8) 0.065(3) Uani 1 1 d . . . H202 H -0.0998 0.3097 0.0762 0.078 Uiso 1 1 calc R . . C203 C -0.0540(7) 0.2565(5) 0.1618(10) 0.083(4) Uani 1 1 d . . . H203 H -0.0880 0.2324 0.1524 0.100 Uiso 1 1 calc R . . C204 C 0.0039(7) 0.2451(5) 0.2229(10) 0.086(4) Uani 1 1 d . . . H204 H 0.0084 0.2136 0.2540 0.103 Uiso 1 1 calc R . . C205 C 0.0535(5) 0.2802(4) 0.2369(8) 0.064(3) Uani 1 1 d . . . H205 H 0.0918 0.2729 0.2784 0.077 Uiso 1 1 calc R . . C206 C 0.1563(5) 0.3738(4) 0.1034(7) 0.043(2) Uani 1 1 d . . . C207 C 0.1316(6) 0.3513(4) 0.0190(7) 0.054(3) Uani 1 1 d . . . H207 H 0.0911 0.3345 0.0108 0.065 Uiso 1 1 calc R . . C208 C 0.1670(7) 0.3538(5) -0.0516(9) 0.078(4) Uani 1 1 d . . . H208 H 0.1504 0.3385 -0.1085 0.094 Uiso 1 1 calc R . . C209 C 0.2261(7) 0.3783(5) -0.0415(9) 0.074(4) Uani 1 1 d . . . H209 H 0.2498 0.3794 -0.0910 0.089 Uiso 1 1 calc R . . C210 C 0.2505(6) 0.4010(5) 0.0401(10) 0.080(4) Uani 1 1 d . . . H210 H 0.2907 0.4182 0.0466 0.095 Uiso 1 1 calc R . . C211 C 0.2164(5) 0.3991(4) 0.1140(8) 0.058(3) Uani 1 1 d . . . H211 H 0.2335 0.4146 0.1706 0.070 Uiso 1 1 calc R . . C212 C 0.1698(5) 0.3682(4) 0.3043(7) 0.048(3) Uani 1 1 d . . . C213 C 0.2077(5) 0.3226(5) 0.3141(8) 0.062(3) Uani 1 1 d . . . H213 H 0.2017 0.2974 0.2678 0.074 Uiso 1 1 calc R . . C214 C 0.2537(5) 0.3159(6) 0.3929(9) 0.077(4) Uani 1 1 d . . . H214 H 0.2779 0.2853 0.4014 0.092 Uiso 1 1 calc R . . C215 C 0.2642(5) 0.3548(6) 0.4605(8) 0.071(4) Uani 1 1 d . . . H215 H 0.2968 0.3507 0.5124 0.085 Uiso 1 1 calc R . . C216 C 0.2268(6) 0.3988(6) 0.4508(8) 0.070(4) Uani 1 1 d . . . H216 H 0.2328 0.4242 0.4968 0.084 Uiso 1 1 calc R . . C217 C 0.1798(5) 0.4051(4) 0.3717(7) 0.053(3) Uani 1 1 d . . . H217 H 0.1547 0.4352 0.3646 0.063 Uiso 1 1 calc R . . C218 C 0.0716(4) 0.4377(4) 0.1981(6) 0.042(2) Uani 1 1 d . . . C219 C 0.0352(5) 0.4500(4) 0.2682(8) 0.054(3) Uani 1 1 d . . . H219 H 0.0324 0.4267 0.3162 0.065 Uiso 1 1 calc R . . C220 C 0.0037(5) 0.4968(6) 0.2654(11) 0.078(4) Uani 1 1 d . . . H220 H -0.0199 0.5054 0.3129 0.094 Uiso 1 1 calc R . . C221 C 0.0060(6) 0.5313(6) 0.1940(13) 0.092(5) Uani 1 1 d . . . H221 H -0.0164 0.5626 0.1929 0.110 Uiso 1 1 calc R . . C222 C 0.0415(6) 0.5196(4) 0.1243(11) 0.072(4) Uani 1 1 d . . . H222 H 0.0433 0.5431 0.0761 0.086 Uiso 1 1 calc R . . C223 C 0.0736(5) 0.4741(4) 0.1259(8) 0.055(3) Uani 1 1 d . . . H223 H 0.0976 0.4665 0.0784 0.066 Uiso 1 1 calc R . . C30 C 0.1985(3) 0.7819(3) 0.1101(8) 0.094(5) Uani 1 1 d G . . H30A H 0.2280 0.7801 0.1706 0.112 Uiso 1 1 d G . . H30B H 0.2154 0.8091 0.0721 0.112 Uiso 1 1 d G . . Cl30 Cl 0.2228(3) 0.7290(2) 0.0615(5) 0.179(2) Uani 1 1 d G . . Cl31 Cl 0.1312(3) 0.8066(3) 0.1276(8) 0.363(7) Uani 1 1 d G . . 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 Mo1 0.0339(4) 0.0393(5) 0.0261(4) -0.0034(4) 0.0064(3) 0.0028(4) Mo2 0.0316(4) 0.0363(5) 0.0282(4) 0.0023(3) 0.0079(3) 0.0049(3) Mo3 0.0311(4) 0.0374(5) 0.0236(4) -0.0002(3) 0.0060(3) 0.0059(3) S1 0.0322(12) 0.0378(13) 0.0295(13) 0.0019(10) 0.0054(10) 0.0059(10) S2 0.0440(14) 0.0532(16) 0.0290(13) 0.0044(11) 0.0052(11) 0.0074(12) S3 0.0498(15) 0.0522(15) 0.0306(14) -0.0014(11) 0.0136(11) 0.0048(12) S4 0.0328(12) 0.0503(15) 0.0368(14) -0.0032(11) 0.0047(10) 0.0076(11) S5 0.0383(13) 0.0479(15) 0.0392(14) 0.0012(11) 0.0133(11) 0.0007(11) S6 0.0444(14) 0.0408(14) 0.0351(14) 0.0040(11) 0.0078(11) 0.0102(11) S7 0.0418(14) 0.0436(14) 0.0393(15) -0.0051(11) 0.0044(11) 0.0006(11) Cl1 0.085(2) 0.0480(16) 0.070(2) -0.0048(14) 0.0204(16) 0.0064(15) Cl2 0.134(3) 0.0521(18) 0.078(2) -0.0177(16) 0.035(2) -0.0254(19) Cl3 0.112(3) 0.104(3) 0.076(2) -0.037(2) 0.006(2) -0.046(2) Cl4 0.0679(19) 0.111(3) 0.0515(18) -0.0238(18) -0.0099(15) 0.0009(18) Cl5 0.0623(17) 0.0567(16) 0.0583(17) 0.0013(13) 0.0240(14) 0.0234(13) Cl6 0.0713(18) 0.0712(18) 0.0436(16) -0.0129(14) 0.0306(14) 0.0052(15) Cl7 0.089(2) 0.0652(18) 0.0299(14) 0.0033(13) 0.0128(13) 0.0013(15) Cl8 0.0577(16) 0.0544(16) 0.0390(14) 0.0099(12) 0.0015(12) 0.0154(12) Cl9 0.0424(14) 0.0479(15) 0.0593(17) 0.0071(12) 0.0122(12) 0.0120(11) Cl10 0.0409(14) 0.0675(18) 0.0619(18) -0.0068(14) 0.0194(13) -0.0082(12) Cl11 0.0763(19) 0.0558(17) 0.0563(18) 0.0075(14) 0.0202(15) -0.0212(14) Cl12 0.0728(18) 0.0415(15) 0.0569(17) 0.0130(13) 0.0131(14) 0.0075(13) O1 0.050(4) 0.042(4) 0.037(4) -0.006(3) 0.007(3) 0.004(3) O2 0.035(4) 0.059(5) 0.040(4) -0.010(3) 0.000(3) 0.003(3) O3 0.033(3) 0.036(3) 0.043(4) 0.012(3) 0.012(3) 0.003(3) O4 0.036(4) 0.045(4) 0.042(4) 0.010(3) 0.008(3) 0.006(3) O5 0.040(4) 0.055(4) 0.029(4) 0.004(3) 0.010(3) 0.016(3) O6 0.040(3) 0.046(4) 0.027(3) 0.004(3) 0.009(3) 0.016(3) C1 0.053(6) 0.041(6) 0.028(5) -0.003(4) 0.017(5) -0.009(5) C2 0.061(7) 0.047(6) 0.040(6) -0.004(5) 0.020(5) -0.007(5) C3 0.114(10) 0.045(7) 0.044(7) -0.019(6) 0.039(7) -0.019(7) C4 0.076(9) 0.076(9) 0.058(8) -0.009(7) 0.014(7) -0.030(7) C5 0.053(7) 0.082(9) 0.033(6) -0.012(6) 0.007(5) -0.009(6) C6 0.049(6) 0.061(7) 0.029(5) -0.003(5) 0.016(5) -0.002(5) C7 0.037(5) 0.032(5) 0.038(6) -0.004(4) -0.004(4) 0.001(4) C8 0.038(5) 0.040(5) 0.035(6) -0.007(4) 0.012(4) 0.009(4) C9 0.047(6) 0.036(5) 0.037(6) -0.015(4) 0.021(5) -0.003(4) C10 0.052(6) 0.043(6) 0.022(5) -0.007(4) 0.015(4) -0.005(5) C11 0.054(6) 0.036(5) 0.023(5) 0.002(4) 0.004(4) 0.003(4) C12 0.036(5) 0.039(5) 0.029(5) -0.004(4) 0.002(4) 0.006(4) C13 0.050(6) 0.037(5) 0.024(5) -0.001(4) 0.010(4) 0.003(4) C14 0.057(6) 0.041(6) 0.026(5) 0.002(4) 0.016(5) 0.001(5) C15 0.053(6) 0.041(6) 0.033(5) -0.009(5) 0.017(5) -0.018(5) C16 0.036(5) 0.046(6) 0.044(6) -0.012(5) 0.019(5) -0.011(5) C17 0.035(5) 0.039(5) 0.030(5) -0.007(4) 0.010(4) -0.003(4) C18 0.040(5) 0.040(5) 0.027(5) -0.011(4) 0.015(4) -0.001(4) P100 0.0477(15) 0.0432(15) 0.0285(14) 0.0001(11) 0.0024(11) -0.0020(12) C100 0.048(6) 0.040(6) 0.042(6) 0.001(5) 0.006(5) 0.003(5) C101 0.059(8) 0.072(8) 0.073(9) 0.014(7) 0.009(6) -0.006(6) C102 0.045(7) 0.089(10) 0.098(11) 0.000(8) -0.003(7) 0.009(6) C103 0.076(9) 0.103(11) 0.066(9) -0.030(8) 0.018(8) -0.004(8) C104 0.078(9) 0.098(10) 0.043(7) -0.017(7) 0.021(7) -0.022(8) C105 0.057(7) 0.052(7) 0.046(7) -0.001(5) 0.012(5) -0.004(5) C106 0.049(6) 0.042(6) 0.031(5) 0.003(4) 0.003(5) -0.002(5) C107 0.065(7) 0.067(8) 0.047(7) -0.007(6) 0.019(6) -0.025(6) C108 0.107(10) 0.086(9) 0.049(8) 0.000(7) 0.048(8) -0.012(8) C109 0.105(11) 0.073(9) 0.035(7) -0.002(6) 0.004(7) 0.010(8) C110 0.070(8) 0.063(7) 0.030(6) 0.005(5) -0.020(6) 0.009(6) C111 0.043(6) 0.058(7) 0.040(6) 0.003(5) -0.003(5) -0.002(5) C112 0.053(6) 0.036(5) 0.030(5) 0.006(4) 0.003(4) 0.003(5) C113 0.054(6) 0.047(6) 0.040(6) 0.010(5) -0.002(5) 0.009(5) C114 0.092(9) 0.038(6) 0.032(6) 0.013(5) 0.000(6) -0.001(6) C115 0.099(10) 0.050(7) 0.049(7) 0.000(6) 0.000(7) -0.034(7) C116 0.071(8) 0.069(9) 0.052(7) 0.013(6) 0.004(6) -0.012(7) C117 0.072(8) 0.048(7) 0.047(7) -0.003(5) 0.008(6) -0.001(6) C118 0.049(6) 0.030(5) 0.035(5) -0.004(4) 0.002(4) 0.007(4) C119 0.068(7) 0.045(6) 0.029(6) -0.008(5) -0.009(5) 0.018(5) C120 0.070(7) 0.043(6) 0.036(6) -0.008(5) 0.004(5) 0.002(5) C121 0.047(6) 0.049(7) 0.058(7) 0.007(6) 0.003(5) 0.008(5) C122 0.053(6) 0.048(6) 0.052(7) -0.014(5) 0.009(5) 0.002(5) C123 0.044(6) 0.046(6) 0.033(6) -0.001(5) -0.004(4) -0.001(5) P200 0.0393(14) 0.0490(16) 0.0328(14) 0.0041(12) 0.0087(11) -0.0033(12) C200 0.038(6) 0.055(7) 0.061(7) -0.001(6) 0.014(5) -0.010(5) C201 0.045(6) 0.053(7) 0.053(7) 0.001(5) 0.001(5) -0.014(5) C202 0.059(7) 0.073(9) 0.060(8) -0.017(7) -0.002(6) -0.016(6) C203 0.081(10) 0.060(9) 0.108(12) 0.009(8) 0.012(8) -0.033(7) C204 0.093(10) 0.067(9) 0.097(11) 0.029(8) 0.017(9) -0.035(8) C205 0.055(7) 0.067(8) 0.065(8) 0.029(6) -0.005(6) -0.010(6) C206 0.046(6) 0.047(6) 0.038(6) 0.014(5) 0.014(5) 0.006(5) C207 0.085(8) 0.041(6) 0.036(6) 0.002(5) 0.011(6) -0.009(5) C208 0.110(11) 0.074(9) 0.053(8) -0.009(7) 0.022(8) -0.010(8) C209 0.112(11) 0.075(9) 0.043(8) 0.013(7) 0.035(8) 0.034(8) C210 0.074(9) 0.077(9) 0.100(11) 0.037(8) 0.051(8) 0.002(7) C211 0.052(7) 0.078(8) 0.048(7) 0.015(6) 0.015(5) -0.008(6) C212 0.042(6) 0.064(7) 0.041(6) 0.014(6) 0.014(5) -0.009(5) C213 0.048(6) 0.090(9) 0.047(7) 0.019(6) 0.007(5) 0.008(6) C214 0.049(7) 0.102(11) 0.075(9) 0.020(9) 0.001(7) 0.013(7) C215 0.041(7) 0.123(12) 0.047(8) 0.025(8) 0.001(6) -0.011(7) C216 0.057(7) 0.115(11) 0.037(7) 0.004(7) 0.003(6) -0.029(8) C217 0.047(6) 0.064(7) 0.044(7) 0.006(6) -0.001(5) -0.010(5) C218 0.032(5) 0.056(6) 0.037(6) -0.011(5) 0.007(4) -0.010(5) C219 0.046(6) 0.062(7) 0.055(7) -0.015(6) 0.011(5) -0.005(5) C220 0.043(7) 0.098(11) 0.091(11) -0.052(9) 0.003(7) -0.012(7) C221 0.047(8) 0.069(10) 0.149(16) -0.031(11) -0.017(9) -0.002(7) C222 0.061(8) 0.033(7) 0.112(12) -0.002(7) -0.015(8) -0.001(6) C223 0.055(7) 0.055(7) 0.055(7) -0.001(6) 0.007(5) -0.003(5) C30 0.091(10) 0.070(9) 0.139(14) -0.023(9) 0.078(10) -0.002(8) Cl30 0.169(5) 0.183(6) 0.189(6) -0.049(5) 0.038(4) -0.063(4) Cl31 0.249(9) 0.251(10) 0.55(2) 0.010(11) -0.062(11) -0.170(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 Mo1 O1 2.055(6) . ? Mo1 O2 2.107(6) . ? Mo1 S1 2.363(2) . ? Mo1 S2 2.403(3) . ? Mo1 S4 2.406(2) . ? Mo1 S3 2.511(2) . ? Mo1 S5 2.517(2) . ? Mo1 Mo2 2.7526(12) . ? Mo1 Mo3 2.7628(11) . ? Mo2 O3 2.058(5) . ? Mo2 O4 2.108(6) . ? Mo2 S1 2.364(2) . ? Mo2 S2 2.415(3) . ? Mo2 S6 2.416(2) . ? Mo2 S3 2.520(3) . ? Mo2 S7 2.524(3) . ? Mo2 Mo3 2.7631(12) . ? Mo3 O6 2.054(6) . ? Mo3 O5 2.115(5) . ? Mo3 S1 2.369(2) . ? Mo3 S4 2.398(3) . ? Mo3 S6 2.412(2) . ? Mo3 S5 2.508(3) . ? Mo3 S7 2.530(3) . ? S2 S3 2.020(3) . ? S4 S5 2.027(3) . ? S6 S7 2.028(3) . ? Cl1 C2 1.752(11) . ? Cl2 C3 1.743(11) . ? Cl3 C4 1.711(12) . ? Cl4 C5 1.724(11) . ? Cl5 C8 1.711(9) . ? Cl6 C9 1.722(8) . ? Cl7 C10 1.737(9) . ? Cl8 C11 1.739(9) . ? Cl9 C17 1.735(9) . ? Cl10 C16 1.728(9) . ? Cl11 C15 1.720(9) . ? Cl12 C14 1.725(9) . ? O1 C1 1.338(10) . ? O2 C6 1.302(11) . ? O3 C18 1.339(10) . ? O4 C13 1.327(10) . ? O5 C7 1.334(10) . ? O6 C12 1.329(10) . ? C1 C2 1.369(13) . ? C1 C6 1.428(13) . ? C2 C3 1.413(15) . ? C3 C4 1.382(16) . ? C4 C5 1.388(16) . ? C5 C6 1.393(14) . ? C7 C8 1.393(12) . ? C7 C12 1.418(12) . ? C8 C9 1.396(12) . ? C9 C10 1.395(12) . ? C10 C11 1.389(12) . ? C11 C12 1.392(12) . ? C13 C14 1.390(12) . ? C13 C18 1.413(12) . ? C14 C15 1.394(12) . ? C15 C16 1.414(13) . ? C16 C17 1.391(12) . ? C17 C18 1.365(11) . ? P100 C100 1.794(10) . ? P100 C106 1.801(9) . ? P100 C112 1.802(9) . ? P100 C118 1.812(9) . ? C100 C105 1.371(13) . ? C100 C101 1.382(14) . ? C101 C102 1.377(15) . ? C101 H101 0.9300 . ? C102 C103 1.351(17) . ? C102 H102 0.9300 . ? C103 C104 1.365(17) . ? C103 H103 0.9300 . ? C104 C105 1.379(14) . ? C104 H104 0.9300 . ? C105 H105 0.9300 . ? C106 C111 1.376(12) . ? C106 C107 1.379(13) . ? C107 C108 1.382(14) . ? C107 H107 0.9300 . ? C108 C109 1.366(16) . ? C108 H108 0.9300 . ? C109 C110 1.358(15) . ? C109 H109 0.9300 . ? C110 C111 1.373(14) . ? C110 H110 0.9300 . ? C111 H111 0.9300 . ? C112 C117 1.387(13) . ? C112 C113 1.410(12) . ? C113 C114 1.371(13) . ? C113 H113 0.9300 . ? C114 C115 1.378(15) . ? C114 H114 0.9300 . ? C115 C116 1.378(16) . ? C115 H115 0.9300 . ? C116 C117 1.368(14) . ? C116 H116 0.9300 . ? C117 H117 0.9300 . ? C118 C119 1.374(12) . ? C118 C123 1.396(12) . ? C119 C120 1.389(13) . ? C119 H119 0.9300 . ? C120 C121 1.345(13) . ? C120 H120 0.9300 . ? C121 C122 1.387(13) . ? C121 H121 0.9300 . ? C122 C123 1.397(13) . ? C122 H122 0.9300 . ? C123 H123 0.9300 . ? P200 C218 1.789(10) . ? P200 C212 1.793(10) . ? P200 C206 1.794(9) . ? P200 C200 1.798(10) . ? C200 C201 1.397(13) . ? C200 C205 1.421(14) . ? C201 C202 1.362(13) . ? C201 H201 0.9300 . ? C202 C203 1.358(16) . ? C202 H202 0.9300 . ? C203 C204 1.396(17) . ? C203 H203 0.9300 . ? C204 C205 1.355(15) . ? C204 H204 0.9300 . ? C205 H205 0.9300 . ? C206 C207 1.376(13) . ? C206 C211 1.386(13) . ? C207 C208 1.350(15) . ? C207 H207 0.9300 . ? C208 C209 1.358(17) . ? C208 H208 0.9300 . ? C209 C210 1.344(17) . ? C209 H209 0.9300 . ? C210 C211 1.373(15) . ? C210 H210 0.9300 . ? C211 H211 0.9300 . ? C212 C217 1.358(14) . ? C212 C213 1.407(14) . ? C213 C214 1.373(15) . ? C213 H213 0.9300 . ? C214 C215 1.396(17) . ? C214 H214 0.9300 . ? C215 C216 1.368(17) . ? C215 H215 0.9300 . ? C216 C217 1.386(14) . ? C216 H216 0.9300 . ? C217 H217 0.9300 . ? C218 C219 1.393(13) . ? C218 C223 1.414(14) . ? C219 C220 1.370(16) . ? C219 H219 0.9300 . ? C220 C221 1.374(19) . ? C220 H220 0.9300 . ? C221 C222 1.372(19) . ? C221 H221 0.9300 . ? C222 C223 1.348(14) . ? C222 H222 0.9300 . ? C223 H223 0.9300 . ? C30 Cl31 1.5809 . ? C30 Cl30 1.6502 . ? C30 H30A 0.9862 . ? C30 H30B 0.9916 . ? 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 O1 Mo1 O2 77.6(2) . . ? O1 Mo1 S1 82.95(18) . . ? O2 Mo1 S1 160.49(19) . . ? O1 Mo1 S2 133.32(18) . . ? O2 Mo1 S2 85.08(19) . . ? S1 Mo1 S2 109.40(9) . . ? O1 Mo1 S4 136.46(18) . . ? O2 Mo1 S4 85.28(18) . . ? S1 Mo1 S4 108.75(8) . . ? S2 Mo1 S4 83.50(9) . . ? O1 Mo1 S3 89.40(18) . . ? O2 Mo1 S3 93.51(18) . . ? S1 Mo1 S3 87.11(8) . . ? S2 Mo1 S3 48.48(8) . . ? S4 Mo1 S3 131.77(9) . . ? O1 Mo1 S5 92.54(18) . . ? O2 Mo1 S5 93.55(18) . . ? S1 Mo1 S5 86.38(8) . . ? S2 Mo1 S5 131.90(8) . . ? S4 Mo1 S5 48.58(8) . . ? S3 Mo1 S5 172.93(9) . . ? O1 Mo1 Mo2 123.36(17) . . ? O2 Mo1 Mo2 139.94(19) . . ? S1 Mo1 Mo2 54.41(6) . . ? S2 Mo1 Mo2 55.36(7) . . ? S4 Mo1 Mo2 95.21(7) . . ? S3 Mo1 Mo2 56.98(6) . . ? S5 Mo1 Mo2 116.59(7) . . ? O1 Mo1 Mo3 125.28(17) . . ? O2 Mo1 Mo3 139.46(17) . . ? S1 Mo1 Mo3 54.37(6) . . ? S2 Mo1 Mo3 95.62(7) . . ? S4 Mo1 Mo3 54.75(6) . . ? S3 Mo1 Mo3 117.10(7) . . ? S5 Mo1 Mo3 56.49(6) . . ? Mo2 Mo1 Mo3 60.13(3) . . ? O3 Mo2 O4 77.8(2) . . ? O3 Mo2 S1 82.57(16) . . ? O4 Mo2 S1 160.31(17) . . ? O3 Mo2 S2 134.10(18) . . ? O4 Mo2 S2 85.66(18) . . ? S1 Mo2 S2 108.96(9) . . ? O3 Mo2 S6 135.53(18) . . ? O4 Mo2 S6 85.09(17) . . ? S1 Mo2 S6 108.95(8) . . ? S2 Mo2 S6 83.99(8) . . ? O3 Mo2 S3 90.15(18) . . ? O4 Mo2 S3 93.82(18) . . ? S1 Mo2 S3 86.88(8) . . ? S2 Mo2 S3 48.27(8) . . ? S6 Mo2 S3 132.08(9) . . ? O3 Mo2 S7 91.59(18) . . ? O4 Mo2 S7 93.14(18) . . ? S1 Mo2 S7 86.67(8) . . ? S2 Mo2 S7 132.21(8) . . ? S6 Mo2 S7 48.41(8) . . ? S3 Mo2 S7 173.04(9) . . ? O3 Mo2 Mo1 123.39(16) . . ? O4 Mo2 Mo1 140.09(17) . . ? S1 Mo2 Mo1 54.37(6) . . ? S2 Mo2 Mo1 54.96(6) . . ? S6 Mo2 Mo1 95.74(7) . . ? S3 Mo2 Mo1 56.67(6) . . ? S7 Mo2 Mo1 117.06(7) . . ? O3 Mo2 Mo3 124.62(16) . . ? O4 Mo2 Mo3 139.58(16) . . ? S1 Mo2 Mo3 54.35(6) . . ? S2 Mo2 Mo3 95.34(6) . . ? S6 Mo2 Mo3 55.02(6) . . ? S3 Mo2 Mo3 116.77(6) . . ? S7 Mo2 Mo3 56.97(6) . . ? Mo1 Mo2 Mo3 60.12(3) . . ? O6 Mo3 O5 77.7(2) . . ? O6 Mo3 S1 83.92(16) . . ? O5 Mo3 S1 161.56(17) . . ? O6 Mo3 S4 133.60(18) . . ? O5 Mo3 S4 83.14(17) . . ? S1 Mo3 S4 108.83(8) . . ? O6 Mo3 S6 135.37(18) . . ? O5 Mo3 S6 85.81(18) . . ? S1 Mo3 S6 108.92(8) . . ? S4 Mo3 S6 83.82(9) . . ? O6 Mo3 S5 89.72(18) . . ? O5 Mo3 S5 91.64(18) . . ? S1 Mo3 S5 86.46(8) . . ? S4 Mo3 S5 48.76(8) . . ? S6 Mo3 S5 132.38(9) . . ? O6 Mo3 S7 92.13(18) . . ? O5 Mo3 S7 95.95(18) . . ? S1 Mo3 S7 86.42(8) . . ? S4 Mo3 S7 131.94(9) . . ? S6 Mo3 S7 48.37(8) . . ? S5 Mo3 S7 172.41(8) . . ? O6 Mo3 Mo1 124.31(17) . . ? O5 Mo3 Mo1 137.53(17) . . ? S1 Mo3 Mo1 54.18(6) . . ? S4 Mo3 Mo1 55.02(6) . . ? S6 Mo3 Mo1 95.56(7) . . ? S5 Mo3 Mo1 56.80(6) . . ? S7 Mo3 Mo1 116.46(7) . . ? O6 Mo3 Mo2 125.79(16) . . ? O5 Mo3 Mo2 140.75(17) . . ? S1 Mo3 Mo2 54.20(6) . . ? S4 Mo3 Mo2 95.12(7) . . ? S6 Mo3 Mo2 55.14(6) . . ? S5 Mo3 Mo2 116.52(6) . . ? S7 Mo3 Mo2 56.74(6) . . ? Mo1 Mo3 Mo2 59.75(3) . . ? Mo1 S1 Mo2 71.23(7) . . ? Mo1 S1 Mo3 71.45(6) . . ? Mo2 S1 Mo3 71.44(7) . . ? S3 S2 Mo1 68.54(10) . . ? S3 S2 Mo2 68.58(10) . . ? Mo1 S2 Mo2 69.68(7) . . ? S2 S3 Mo1 62.98(9) . . ? S2 S3 Mo2 63.15(10) . . ? Mo1 S3 Mo2 66.35(6) . . ? S5 S4 Mo3 68.46(10) . . ? S5 S4 Mo1 68.57(9) . . ? Mo3 S4 Mo1 70.22(7) . . ? S4 S5 Mo3 62.78(10) . . ? S4 S5 Mo1 62.84(9) . . ? Mo3 S5 Mo1 66.71(6) . . ? S7 S6 Mo3 68.87(10) . . ? S7 S6 Mo2 68.58(10) . . ? Mo3 S6 Mo2 69.83(7) . . ? S6 S7 Mo2 63.01(9) . . ? S6 S7 Mo3 62.76(9) . . ? Mo2 S7 Mo3 66.29(7) . . ? C1 O1 Mo1 115.2(6) . . ? C6 O2 Mo1 114.1(6) . . ? C18 O3 Mo2 114.6(5) . . ? C13 O4 Mo2 114.0(5) . . ? C7 O5 Mo3 113.2(5) . . ? C12 O6 Mo3 115.1(5) . . ? O1 C1 C2 125.1(9) . . ? O1 C1 C6 115.8(8) . . ? C2 C1 C6 119.0(9) . . ? C1 C2 C3 121.4(10) . . ? C1 C2 Cl1 117.8(8) . . ? C3 C2 Cl1 120.8(8) . . ? C4 C3 C2 119.9(10) . . ? C4 C3 Cl2 121.3(10) . . ? C2 C3 Cl2 118.8(10) . . ? C3 C4 C5 118.9(11) . . ? C3 C4 Cl3 118.7(10) . . ? C5 C4 Cl3 122.2(11) . . ? C4 C5 C6 122.2(11) . . ? C4 C5 Cl4 119.3(9) . . ? C6 C5 Cl4 118.6(9) . . ? O2 C6 C5 124.3(10) . . ? O2 C6 C1 117.2(9) . . ? C5 C6 C1 118.5(10) . . ? O5 C7 C8 122.6(8) . . ? O5 C7 C12 116.5(8) . . ? C8 C7 C12 120.9(8) . . ? C7 C8 C9 119.7(8) . . ? C7 C8 Cl5 119.6(7) . . ? C9 C8 Cl5 120.6(6) . . ? C10 C9 C8 120.0(7) . . ? C10 C9 Cl6 119.0(7) . . ? C8 C9 Cl6 121.0(7) . . ? C11 C10 C9 119.9(8) . . ? C11 C10 Cl7 119.4(7) . . ? C9 C10 Cl7 120.6(6) . . ? C10 C11 C12 121.4(8) . . ? C10 C11 Cl8 121.7(7) . . ? C12 C11 Cl8 116.8(7) . . ? O6 C12 C11 125.0(8) . . ? O6 C12 C7 117.0(8) . . ? C11 C12 C7 118.0(8) . . ? O4 C13 C14 125.3(8) . . ? O4 C13 C18 116.2(8) . . ? C14 C13 C18 118.5(8) . . ? C13 C14 C15 121.4(9) . . ? C13 C14 Cl12 118.2(7) . . ? C15 C14 Cl12 120.4(7) . . ? C14 C15 C16 119.0(8) . . ? C14 C15 Cl11 120.8(8) . . ? C16 C15 Cl11 120.2(7) . . ? C17 C16 C15 119.3(8) . . ? C17 C16 Cl10 121.9(8) . . ? C15 C16 Cl10 118.8(7) . . ? C18 C17 C16 121.3(9) . . ? C18 C17 Cl9 119.8(7) . . ? C16 C17 Cl9 118.8(7) . . ? O3 C18 C17 122.2(8) . . ? O3 C18 C13 117.4(7) . . ? C17 C18 C13 120.4(8) . . ? C100 P100 C106 110.5(5) . . ? C100 P100 C112 107.3(4) . . ? C106 P100 C112 114.3(4) . . ? C100 P100 C118 111.1(4) . . ? C106 P100 C118 105.5(4) . . ? C112 P100 C118 108.0(4) . . ? C105 C100 C101 119.5(10) . . ? C105 C100 P100 119.0(8) . . ? C101 C100 P100 120.9(8) . . ? C102 C101 C100 119.8(11) . . ? C102 C101 H101 120.1 . . ? C100 C101 H101 120.1 . . ? C103 C102 C101 120.5(12) . . ? C103 C102 H102 119.8 . . ? C101 C102 H102 119.8 . . ? C102 C103 C104 120.0(12) . . ? C102 C103 H103 120.0 . . ? C104 C103 H103 120.0 . . ? C103 C104 C105 120.6(11) . . ? C103 C104 H104 119.7 . . ? C105 C104 H104 119.7 . . ? C100 C105 C104 119.6(10) . . ? C100 C105 H105 120.2 . . ? C104 C105 H105 120.2 . . ? C111 C106 C107 119.3(9) . . ? C111 C106 P100 119.7(7) . . ? C107 C106 P100 119.8(8) . . ? C106 C107 C108 119.4(10) . . ? C106 C107 H107 120.3 . . ? C108 C107 H107 120.3 . . ? C109 C108 C107 120.5(11) . . ? C109 C108 H108 119.8 . . ? C107 C108 H108 119.8 . . ? C110 C109 C108 120.2(11) . . ? C110 C109 H109 119.9 . . ? C108 C109 H109 119.9 . . ? C109 C110 C111 119.9(11) . . ? C109 C110 H110 120.0 . . ? C111 C110 H110 120.0 . . ? C110 C111 C106 120.7(10) . . ? C110 C111 H111 119.7 . . ? C106 C111 H111 119.7 . . ? C117 C112 C113 119.8(9) . . ? C117 C112 P100 120.1(7) . . ? C113 C112 P100 120.1(8) . . ? C114 C113 C112 118.4(10) . . ? C114 C113 H113 120.8 . . ? C112 C113 H113 120.8 . . ? C113 C114 C115 120.8(11) . . ? C113 C114 H114 119.6 . . ? C115 C114 H114 119.6 . . ? C116 C115 C114 121.0(11) . . ? C116 C115 H115 119.5 . . ? C114 C115 H115 119.5 . . ? C117 C116 C115 119.0(11) . . ? C117 C116 H116 120.5 . . ? C115 C116 H116 120.5 . . ? C116 C117 C112 120.8(10) . . ? C116 C117 H117 119.6 . . ? C112 C117 H117 119.6 . . ? C119 C118 C123 120.8(8) . . ? C119 C118 P100 121.0(7) . . ? C123 C118 P100 118.2(7) . . ? C118 C119 C120 118.8(9) . . ? C118 C119 H119 120.6 . . ? C120 C119 H119 120.6 . . ? C121 C120 C119 122.1(10) . . ? C121 C120 H120 119.0 . . ? C119 C120 H120 119.0 . . ? C120 C121 C122 119.3(10) . . ? C120 C121 H121 120.3 . . ? C122 C121 H121 120.3 . . ? C121 C122 C123 120.6(9) . . ? C121 C122 H122 119.7 . . ? C123 C122 H122 119.7 . . ? C118 C123 C122 118.3(9) . . ? C118 C123 H123 120.8 . . ? C122 C123 H123 120.8 . . ? C218 P200 C212 110.6(5) . . ? C218 P200 C206 108.2(4) . . ? C212 P200 C206 107.2(4) . . ? C218 P200 C200 106.6(4) . . ? C212 P200 C200 112.4(5) . . ? C206 P200 C200 111.8(5) . . ? C201 C200 C205 118.7(9) . . ? C201 C200 P200 118.2(8) . . ? C205 C200 P200 123.1(8) . . ? C202 C201 C200 119.7(10) . . ? C202 C201 H201 120.1 . . ? C200 C201 H201 120.1 . . ? C203 C202 C201 121.4(11) . . ? C203 C202 H202 119.3 . . ? C201 C202 H202 119.3 . . ? C202 C203 C204 120.2(11) . . ? C202 C203 H203 119.9 . . ? C204 C203 H203 119.9 . . ? C205 C204 C203 120.0(11) . . ? C205 C204 H204 120.0 . . ? C203 C204 H204 120.0 . . ? C204 C205 C200 120.0(10) . . ? C204 C205 H205 120.0 . . ? C200 C205 H205 120.0 . . ? C207 C206 C211 119.6(9) . . ? C207 C206 P200 122.8(8) . . ? C211 C206 P200 117.4(8) . . ? C208 C207 C206 119.1(11) . . ? C208 C207 H207 120.4 . . ? C206 C207 H207 120.4 . . ? C207 C208 C209 121.6(12) . . ? C207 C208 H208 119.2 . . ? C209 C208 H208 119.2 . . ? C210 C209 C208 119.9(12) . . ? C210 C209 H209 120.1 . . ? C208 C209 H209 120.1 . . ? C209 C210 C211 120.6(12) . . ? C209 C210 H210 119.7 . . ? C211 C210 H210 119.7 . . ? C210 C211 C206 119.2(11) . . ? C210 C211 H211 120.4 . . ? C206 C211 H211 120.4 . . ? C217 C212 C213 119.9(10) . . ? C217 C212 P200 122.3(8) . . ? C213 C212 P200 117.7(8) . . ? C214 C213 C212 119.1(12) . . ? C214 C213 H213 120.4 . . ? C212 C213 H213 120.4 . . ? C213 C214 C215 120.1(12) . . ? C213 C214 H214 120.0 . . ? C215 C214 H214 120.0 . . ? C216 C215 C214 120.3(11) . . ? C216 C215 H215 119.8 . . ? C214 C215 H215 119.8 . . ? C215 C216 C217 119.3(12) . . ? C215 C216 H216 120.3 . . ? C217 C216 H216 120.3 . . ? C212 C217 C216 121.2(11) . . ? C212 C217 H217 119.4 . . ? C216 C217 H217 119.4 . . ? C219 C218 C223 118.2(10) . . ? C219 C218 P200 119.5(8) . . ? C223 C218 P200 122.2(7) . . ? C220 C219 C218 119.2(11) . . ? C220 C219 H219 120.4 . . ? C218 C219 H219 120.4 . . ? C219 C220 C221 121.4(13) . . ? C219 C220 H220 119.3 . . ? C221 C220 H220 119.3 . . ? C222 C221 C220 120.1(13) . . ? C222 C221 H221 120.0 . . ? C220 C221 H221 120.0 . . ? C223 C222 C221 119.8(13) . . ? C223 C222 H222 120.1 . . ? C221 C222 H222 120.1 . . ? C222 C223 C218 121.4(11) . . ? C222 C223 H223 119.3 . . ? C218 C223 H223 119.3 . . ? Cl31 C30 Cl30 137.4 . . ? Cl31 C30 H30A 107.8 . . ? Cl30 C30 H30A 99.0 . . ? Cl31 C30 H30B 101.4 . . ? Cl30 C30 H30B 101.0 . . ? H30A C30 H30B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.145 _refine_diff_density_min -1.178 _refine_diff_density_rms 0.140 #===END data_(PPh4)2[3] _database_code_depnum_ccdc_archive 'CCDC 713963' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '4(C24 H20 P), 2(I6 Mo3 S7), C Cl2' _chemical_formula_sum 'C48.50 H41 Cl I6 Mo3 P2 S7' _chemical_formula_weight 1994.84 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' P P 0.1023 0.0942 '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' Mo Mo -1.6832 0.6857 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 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 18.5189(10) _cell_length_b 20.9106(11) _cell_length_c 17.2686(9) _cell_angle_alpha 90.00 _cell_angle_beta 106.8220(10) _cell_angle_gamma 90.00 _cell_volume 6401.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6949 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 30.45 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.070 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3740 _exptl_absorpt_coefficient_mu 3.824 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6167 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'Bruker SADABS' _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_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42209 _diffrn_reflns_av_R_equivalents 0.0454 _diffrn_reflns_av_sigmaI/netI 0.0518 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 27.50 _reflns_number_total 14670 _reflns_number_gt 10793 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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 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^)+(0.0567P)^2^+7.8517P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14670 _refine_ls_number_parameters 598 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.1291 _refine_ls_wR_factor_gt 0.1040 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.165 _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 Mo1 Mo 0.20883(3) 0.55530(2) 0.45181(3) 0.02751(11) Uani 1 1 d . . . Mo2 Mo 0.14203(3) 0.46222(2) 0.34156(3) 0.02727(11) Uani 1 1 d . . . Mo3 Mo 0.05693(3) 0.56176(2) 0.37226(3) 0.02538(11) Uani 1 1 d . . . S1 S 0.15504(9) 0.57063(7) 0.31191(9) 0.0303(3) Uani 1 1 d . . . S2 S 0.27948(9) 0.46543(8) 0.41379(10) 0.0388(4) Uani 1 1 d . . . S3 S 0.20814(9) 0.44345(7) 0.48000(9) 0.0343(3) Uani 1 1 d . . . S4 S 0.00583(9) 0.47748(8) 0.26957(9) 0.0347(3) Uani 1 1 d . . . S5 S 0.03246(9) 0.45037(7) 0.38746(9) 0.0305(3) Uani 1 1 d . . . S6 S 0.12652(9) 0.64633(7) 0.46641(10) 0.0340(3) Uani 1 1 d . . . S7 S 0.11075(9) 0.56144(7) 0.51692(9) 0.0301(3) Uani 1 1 d . . . I1 I 0.31431(3) 0.64259(2) 0.42175(3) 0.04713(13) Uani 1 1 d . . . I2 I 0.30979(3) 0.55728(3) 0.61424(3) 0.04973(13) Uani 1 1 d . . . I3 I 0.17440(3) 0.44948(2) 0.19240(3) 0.04739(13) Uani 1 1 d . . . I4 I 0.13615(3) 0.32530(2) 0.33302(3) 0.04634(12) Uani 1 1 d . . . I5 I -0.00491(3) 0.65650(2) 0.25700(3) 0.04186(11) Uani 1 1 d . . . I6 I -0.08609(2) 0.57882(2) 0.40591(3) 0.03865(11) Uani 1 1 d . . . P100 P 0.39544(11) 0.21843(11) 0.49380(13) 0.0514(5) Uani 1 1 d . . . P200 P 0.85864(10) 0.36459(8) 0.04073(10) 0.0349(4) Uani 1 1 d . . . C100 C 0.4830(5) 0.1889(4) 0.5607(5) 0.060(2) Uani 1 1 d . . . C101 C 0.5425(6) 0.1731(7) 0.5301(8) 0.102(4) Uani 1 1 d . . . H101 H 0.5381 0.1785 0.4755 0.122 Uiso 1 1 calc R . . C102 C 0.6079(6) 0.1492(7) 0.5824(9) 0.108(4) Uani 1 1 d . . . H102 H 0.6480 0.1383 0.5628 0.129 Uiso 1 1 calc R . . C103 C 0.6144(6) 0.1414(6) 0.6620(8) 0.096(4) Uani 1 1 d . . . H103 H 0.6589 0.1249 0.6963 0.115 Uiso 1 1 calc R . . C104 C 0.5573(6) 0.1573(6) 0.6919(7) 0.092(3) Uani 1 1 d . . . H104 H 0.5631 0.1526 0.7469 0.110 Uiso 1 1 calc R . . C105 C 0.4908(5) 0.1803(5) 0.6422(6) 0.072(3) Uani 1 1 d . . . H105 H 0.4511 0.1900 0.6630 0.086 Uiso 1 1 calc R . . C106 C 0.4162(4) 0.2831(4) 0.4346(5) 0.057(2) Uani 1 1 d . . . C107 C 0.4799(6) 0.3175(7) 0.4644(8) 0.132(6) Uani 1 1 d D . . H107 H 0.5143 0.3054 0.5130 0.158 Uiso 1 1 calc R . . C108 C 0.4949(7) 0.3711(7) 0.4231(9) 0.151(8) Uani 1 1 d D . . H108 H 0.5371 0.3963 0.4454 0.181 Uiso 1 1 calc R . . C109 C 0.4454(6) 0.3858(6) 0.3482(7) 0.109(5) Uani 1 1 d D . . H109 H 0.4574 0.4180 0.3169 0.131 Uiso 1 1 calc R . . C110 C 0.3781(5) 0.3528(4) 0.3199(6) 0.075(3) Uani 1 1 d D . . H110 H 0.3423 0.3653 0.2724 0.090 Uiso 1 1 calc R . . C111 C 0.3656(5) 0.3008(4) 0.3639(5) 0.072(3) Uani 1 1 d D . . H111 H 0.3213 0.2774 0.3445 0.086 Uiso 1 1 calc R . . C112 C 0.3379(4) 0.2465(4) 0.5541(5) 0.0531(19) Uani 1 1 d . . . C113 C 0.3356(5) 0.3100(4) 0.5724(6) 0.065(2) Uani 1 1 d . . . H113 H 0.3609 0.3399 0.5500 0.078 Uiso 1 1 calc R . . C114 C 0.2948(6) 0.3298(5) 0.6251(6) 0.078(3) Uani 1 1 d . . . H114 H 0.2937 0.3727 0.6387 0.094 Uiso 1 1 calc R . . C115 C 0.2568(5) 0.2859(5) 0.6564(5) 0.066(2) Uani 1 1 d . . . H115 H 0.2289 0.2995 0.6902 0.079 Uiso 1 1 calc R . . C116 C 0.2589(5) 0.2214(5) 0.6387(6) 0.068(2) Uani 1 1 d . . . H116 H 0.2339 0.1915 0.6616 0.082 Uiso 1 1 calc R . . C117 C 0.2986(4) 0.2026(4) 0.5868(5) 0.0556(19) Uani 1 1 d . . . H117 H 0.2993 0.1596 0.5733 0.067 Uiso 1 1 calc R . . C118 C 0.3449(5) 0.1568(4) 0.4266(5) 0.0563(19) Uani 1 1 d . . . C119 C 0.2695(5) 0.1663(4) 0.3839(5) 0.059(2) Uani 1 1 d . . . H119 H 0.2446 0.2029 0.3929 0.071 Uiso 1 1 calc R . . C120 C 0.2318(6) 0.1216(5) 0.3282(6) 0.073(3) Uani 1 1 d . . . H120 H 0.1812 0.1282 0.3005 0.088 Uiso 1 1 calc R . . C121 C 0.2669(8) 0.0682(6) 0.3129(7) 0.091(3) Uani 1 1 d . . . H121 H 0.2415 0.0392 0.2736 0.109 Uiso 1 1 calc R . . C122 C 0.3400(8) 0.0578(6) 0.3562(9) 0.115(5) Uani 1 1 d . . . H122 H 0.3641 0.0205 0.3477 0.138 Uiso 1 1 calc R . . C123 C 0.3800(6) 0.1028(6) 0.4139(8) 0.092(4) Uani 1 1 d . . . H123 H 0.4301 0.0954 0.4429 0.111 Uiso 1 1 calc R . . C200 C 0.8425(4) 0.3477(3) 0.1361(4) 0.0366(14) Uani 1 1 d . . . C201 C 0.8442(5) 0.2848(4) 0.1638(4) 0.0498(18) Uani 1 1 d . . . H201 H 0.8524 0.2511 0.1322 0.060 Uiso 1 1 calc R . . C202 C 0.8335(5) 0.2727(4) 0.2390(5) 0.061(2) Uani 1 1 d . . . H202 H 0.8339 0.2308 0.2571 0.073 Uiso 1 1 calc R . . C203 C 0.8225(4) 0.3222(4) 0.2866(5) 0.056(2) Uani 1 1 d . . . H203 H 0.8148 0.3138 0.3365 0.067 Uiso 1 1 calc R . . C204 C 0.8229(4) 0.3836(4) 0.2605(5) 0.0526(19) Uani 1 1 d . . . H204 H 0.8168 0.4171 0.2935 0.063 Uiso 1 1 calc R . . C205 C 0.8323(4) 0.3967(3) 0.1854(4) 0.0426(15) Uani 1 1 d . . . H205 H 0.8316 0.4389 0.1681 0.051 Uiso 1 1 calc R . . C206 C 0.8752(5) 0.4486(3) 0.0379(4) 0.0432(16) Uani 1 1 d . . . C207 C 0.8127(5) 0.4897(3) 0.0154(4) 0.056(2) Uani 1 1 d . . . H207 H 0.7638 0.4737 -0.0024 0.067 Uiso 1 1 calc R . . C208 C 0.8266(8) 0.5559(4) 0.0208(5) 0.078(3) Uani 1 1 d . . . H208 H 0.7864 0.5842 0.0044 0.093 Uiso 1 1 calc R . . C209 C 0.8984(8) 0.5791(4) 0.0497(6) 0.080(3) Uani 1 1 d . . . H209 H 0.9062 0.6230 0.0546 0.096 Uiso 1 1 calc R . . C210 C 0.9593(6) 0.5382(4) 0.0718(5) 0.072(3) Uani 1 1 d . . . H210 H 1.0081 0.5543 0.0908 0.086 Uiso 1 1 calc R . . C211 C 0.9469(5) 0.4723(4) 0.0651(5) 0.0521(19) Uani 1 1 d . . . H211 H 0.9877 0.4443 0.0793 0.063 Uiso 1 1 calc R . . C212 C 0.7801(4) 0.3430(3) -0.0436(4) 0.0398(15) Uani 1 1 d . . . C213 C 0.7350(4) 0.2911(4) -0.0381(5) 0.0520(18) Uani 1 1 d . . . H213 H 0.7406 0.2712 0.0114 0.062 Uiso 1 1 calc R . . C214 C 0.6818(6) 0.2693(5) -0.1070(6) 0.077(3) Uani 1 1 d . . . H214 H 0.6519 0.2341 -0.1042 0.093 Uiso 1 1 calc R . . C215 C 0.6733(6) 0.2999(6) -0.1801(6) 0.081(3) Uani 1 1 d . . . H215 H 0.6375 0.2852 -0.2263 0.097 Uiso 1 1 calc R . . C216 C 0.7173(5) 0.3518(5) -0.1849(5) 0.068(2) Uani 1 1 d . . . H216 H 0.7114 0.3719 -0.2344 0.082 Uiso 1 1 calc R . . C217 C 0.7700(4) 0.3738(4) -0.1169(4) 0.0506(18) Uani 1 1 d . . . H217 H 0.7990 0.4095 -0.1200 0.061 Uiso 1 1 calc R . . C218 C 0.9381(4) 0.3192(3) 0.0319(4) 0.0371(14) Uani 1 1 d . . . C219 C 0.9402(4) 0.2973(3) -0.0424(4) 0.0440(16) Uani 1 1 d . . . H219 H 0.9006 0.3061 -0.0884 0.053 Uiso 1 1 calc R . . C220 C 1.0020(5) 0.2620(3) -0.0483(5) 0.0492(18) Uani 1 1 d . . . H220 H 1.0032 0.2463 -0.0983 0.059 Uiso 1 1 calc R . . C221 C 1.0606(5) 0.2503(4) 0.0186(5) 0.055(2) Uani 1 1 d . . . H221 H 1.1020 0.2270 0.0143 0.066 Uiso 1 1 calc R . . C222 C 1.0586(4) 0.2731(4) 0.0933(5) 0.057(2) Uani 1 1 d . . . H222 H 1.0988 0.2647 0.1389 0.068 Uiso 1 1 calc R . . C223 C 0.9988(4) 0.3075(3) 0.1011(4) 0.0480(17) Uani 1 1 d . . . H223 H 0.9981 0.3230 0.1514 0.058 Uiso 1 1 calc R . . C300 C 0.5597(4) 0.0565(3) 0.3512(4) 0.155(13) Uiso 0.50 1 d PR . . H30 H 0.5991 0.0890 0.3799 0.186 Uiso 0.50 1 d PR . . H31 H 0.5281 0.0504 0.3897 0.186 Uiso 0.50 1 d PR . . Cl30 Cl 0.6040(4) -0.0139(3) 0.3450(4) 0.433(15) Uiso 0.50 1 d PR . . Cl31 Cl 0.5017(4) 0.0882(3) 0.2639(4) 0.48(2) Uiso 0.50 1 d PR . . 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 Mo1 0.0260(3) 0.0311(2) 0.0255(2) -0.00307(19) 0.0074(2) -0.00258(19) Mo2 0.0299(3) 0.0276(2) 0.0252(2) -0.00243(18) 0.0092(2) -0.00134(19) Mo3 0.0262(3) 0.0253(2) 0.0241(2) 0.00024(18) 0.0065(2) -0.00094(18) S1 0.0327(8) 0.0323(7) 0.0274(7) 0.0007(6) 0.0110(6) -0.0046(6) S2 0.0318(8) 0.0464(9) 0.0392(9) -0.0032(7) 0.0119(7) 0.0031(7) S3 0.0361(8) 0.0355(8) 0.0306(8) 0.0025(6) 0.0088(7) 0.0033(6) S4 0.0345(8) 0.0383(8) 0.0281(8) -0.0012(6) 0.0040(6) -0.0057(6) S5 0.0318(8) 0.0294(7) 0.0323(8) 0.0006(6) 0.0121(6) -0.0027(6) S6 0.0408(9) 0.0276(7) 0.0344(8) -0.0031(6) 0.0122(7) -0.0021(6) S7 0.0320(8) 0.0322(7) 0.0265(7) -0.0002(5) 0.0092(6) -0.0003(6) I1 0.0401(3) 0.0560(3) 0.0454(3) -0.0034(2) 0.0126(2) -0.0177(2) I2 0.0409(3) 0.0730(3) 0.0309(2) -0.0071(2) 0.0034(2) -0.0062(2) I3 0.0672(3) 0.0463(3) 0.0362(2) -0.00488(18) 0.0270(2) 0.0006(2) I4 0.0603(3) 0.0294(2) 0.0521(3) -0.00373(18) 0.0208(2) -0.00086(18) I5 0.0477(3) 0.0373(2) 0.0371(2) 0.00981(17) 0.0068(2) 0.00246(18) I6 0.0345(2) 0.0397(2) 0.0446(2) 0.00920(18) 0.01596(19) 0.00660(17) P100 0.0344(10) 0.0675(13) 0.0482(11) 0.0085(9) 0.0054(9) -0.0015(9) P200 0.0437(10) 0.0336(8) 0.0283(8) -0.0010(6) 0.0121(7) 0.0030(7) C100 0.041(4) 0.069(5) 0.062(5) 0.015(4) 0.004(4) 0.001(4) C101 0.049(6) 0.168(12) 0.088(8) 0.029(8) 0.019(6) 0.027(7) C102 0.042(6) 0.163(13) 0.117(11) 0.039(9) 0.019(6) 0.023(7) C103 0.056(7) 0.109(9) 0.109(10) 0.035(8) 0.002(6) 0.014(6) C104 0.062(7) 0.126(10) 0.068(7) 0.023(6) -0.011(5) 0.018(6) C105 0.051(5) 0.094(7) 0.066(6) 0.021(5) 0.009(4) 0.005(5) C106 0.034(4) 0.076(6) 0.055(5) 0.013(4) 0.005(3) -0.002(4) C107 0.058(7) 0.168(13) 0.131(11) 0.087(10) -0.035(7) -0.059(7) C108 0.067(8) 0.184(15) 0.170(14) 0.105(12) -0.016(9) -0.054(9) C109 0.064(7) 0.149(11) 0.104(9) 0.077(9) 0.010(6) -0.010(7) C110 0.069(6) 0.079(6) 0.067(6) 0.017(5) 0.005(5) 0.000(5) C111 0.068(6) 0.076(6) 0.060(6) 0.011(5) 0.002(5) -0.013(5) C112 0.045(4) 0.064(5) 0.046(4) 0.008(4) 0.006(4) 0.001(4) C113 0.061(6) 0.062(5) 0.071(6) 0.022(4) 0.019(5) 0.014(4) C114 0.088(7) 0.064(6) 0.076(7) 0.005(5) 0.016(6) 0.024(5) C115 0.060(6) 0.080(6) 0.056(5) 0.010(5) 0.014(4) 0.015(5) C116 0.053(5) 0.085(7) 0.066(6) 0.015(5) 0.017(5) -0.006(4) C117 0.046(4) 0.062(5) 0.057(5) 0.003(4) 0.012(4) -0.005(4) C118 0.055(5) 0.063(5) 0.051(5) 0.004(4) 0.015(4) -0.001(4) C119 0.042(4) 0.076(6) 0.054(5) 0.018(4) 0.004(4) -0.003(4) C120 0.062(6) 0.093(7) 0.055(5) 0.016(5) 0.002(5) -0.020(5) C121 0.100(9) 0.093(8) 0.082(8) -0.016(6) 0.029(7) -0.027(7) C122 0.106(11) 0.101(10) 0.138(13) -0.051(9) 0.035(10) -0.002(8) C123 0.055(6) 0.098(8) 0.111(9) -0.012(7) 0.004(6) 0.023(6) C200 0.038(4) 0.040(3) 0.032(3) -0.005(3) 0.011(3) 0.002(3) C201 0.070(5) 0.043(4) 0.041(4) 0.004(3) 0.022(4) 0.007(3) C202 0.079(6) 0.061(5) 0.048(5) 0.015(4) 0.027(4) 0.006(4) C203 0.051(5) 0.087(6) 0.032(4) 0.008(4) 0.016(4) 0.002(4) C204 0.058(5) 0.065(5) 0.041(4) -0.010(4) 0.023(4) 0.000(4) C205 0.041(4) 0.042(4) 0.045(4) -0.005(3) 0.012(3) -0.003(3) C206 0.068(5) 0.032(3) 0.033(3) 0.001(3) 0.021(3) 0.004(3) C207 0.084(6) 0.040(4) 0.041(4) 0.000(3) 0.015(4) 0.015(4) C208 0.142(10) 0.042(5) 0.045(5) 0.004(4) 0.022(6) 0.041(6) C209 0.162(12) 0.037(4) 0.050(5) -0.006(4) 0.044(7) -0.006(6) C210 0.110(8) 0.060(5) 0.059(5) -0.014(4) 0.047(6) -0.034(5) C211 0.071(5) 0.050(4) 0.045(4) -0.009(3) 0.032(4) -0.011(4) C212 0.041(4) 0.042(3) 0.038(4) -0.001(3) 0.014(3) 0.007(3) C213 0.055(5) 0.049(4) 0.049(4) 0.003(3) 0.010(4) -0.005(3) C214 0.069(6) 0.079(6) 0.076(7) -0.006(5) 0.007(5) -0.026(5) C215 0.071(7) 0.103(8) 0.054(6) -0.025(5) -0.004(5) -0.010(6) C216 0.076(6) 0.083(6) 0.038(4) 0.003(4) 0.004(4) 0.004(5) C217 0.054(5) 0.060(5) 0.035(4) -0.003(3) 0.009(3) -0.002(4) C218 0.041(4) 0.030(3) 0.044(4) 0.000(3) 0.019(3) 0.002(3) C219 0.052(4) 0.045(4) 0.037(4) -0.001(3) 0.016(3) 0.008(3) C220 0.066(5) 0.039(4) 0.051(4) -0.003(3) 0.031(4) 0.005(3) C221 0.059(5) 0.049(4) 0.068(5) 0.010(4) 0.035(4) 0.019(4) C222 0.044(4) 0.072(5) 0.052(5) 0.011(4) 0.011(4) 0.018(4) C223 0.054(5) 0.054(4) 0.036(4) 0.001(3) 0.013(3) 0.009(3) _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 S1 2.3533(16) . ? Mo1 S3 2.3899(16) . ? Mo1 S7 2.4005(15) . ? Mo1 S2 2.4842(17) . ? Mo1 S6 2.4965(16) . ? Mo1 Mo2 2.7532(7) . ? Mo1 Mo3 2.7536(7) . ? Mo1 I1 2.8289(7) . ? Mo1 I2 2.8862(7) . ? Mo2 S1 2.3517(15) . ? Mo2 S3 2.3821(16) . ? Mo2 S5 2.3955(15) . ? Mo2 S4 2.4889(17) . ? Mo2 S2 2.4902(17) . ? Mo2 Mo3 2.7533(7) . ? Mo2 I3 2.8212(7) . ? Mo2 I4 2.8674(7) . ? Mo3 S1 2.3490(15) . ? Mo3 S5 2.4017(15) . ? Mo3 S7 2.4069(15) . ? Mo3 S4 2.4849(16) . ? Mo3 S6 2.4939(16) . ? Mo3 I5 2.8069(6) . ? Mo3 I6 2.8931(7) . ? S2 S3 2.034(2) . ? S4 S5 2.032(2) . ? S6 S7 2.036(2) . ? P100 C112 1.791(8) . ? P100 C106 1.802(8) . ? P100 C118 1.805(9) . ? P100 C100 1.806(8) . ? P200 C206 1.786(7) . ? P200 C200 1.792(7) . ? P200 C212 1.793(7) . ? P200 C218 1.794(6) . ? C100 C105 1.384(12) . ? C100 C101 1.391(13) . ? C101 C102 1.378(15) . ? C101 H101 0.9300 . ? C102 C103 1.354(17) . ? C102 H102 0.9300 . ? C103 C104 1.346(16) . ? C103 H103 0.9300 . ? C104 C105 1.368(12) . ? C104 H104 0.9300 . ? C105 H105 0.9300 . ? C106 C107 1.351(12) . ? C106 C111 1.359(11) . ? C107 C108 1.398(11) . ? C107 H107 0.9300 . ? C108 C109 1.386(11) . ? C108 H108 0.9300 . ? C109 C110 1.384(10) . ? C109 H109 0.9300 . ? C110 C111 1.385(10) . ? C110 H110 0.9300 . ? C111 H111 0.9300 . ? C112 C113 1.369(12) . ? C112 C117 1.389(11) . ? C113 C114 1.404(13) . ? C113 H113 0.9300 . ? C114 C115 1.358(13) . ? C114 H114 0.9300 . ? C115 C116 1.386(13) . ? C115 H115 0.9300 . ? C116 C117 1.371(12) . ? C116 H116 0.9300 . ? C117 H117 0.9300 . ? C118 C123 1.351(13) . ? C118 C119 1.392(11) . ? C119 C120 1.378(13) . ? C119 H119 0.9300 . ? C120 C121 1.355(15) . ? C120 H120 0.9300 . ? C121 C122 1.361(17) . ? C121 H121 0.9300 . ? C122 C123 1.414(16) . ? C122 H122 0.9300 . ? C123 H123 0.9300 . ? C200 C205 1.381(9) . ? C200 C201 1.397(9) . ? C201 C202 1.391(10) . ? C201 H201 0.9300 . ? C202 C203 1.372(12) . ? C202 H202 0.9300 . ? C203 C204 1.362(11) . ? C203 H203 0.9300 . ? C204 C205 1.384(10) . ? C204 H204 0.9300 . ? C205 H205 0.9300 . ? C206 C211 1.367(11) . ? C206 C207 1.403(10) . ? C207 C208 1.406(12) . ? C207 H207 0.9300 . ? C208 C209 1.366(15) . ? C208 H208 0.9300 . ? C209 C210 1.379(15) . ? C209 H209 0.9300 . ? C210 C211 1.396(11) . ? C210 H210 0.9300 . ? C211 H211 0.9300 . ? C212 C217 1.383(10) . ? C212 C213 1.389(10) . ? C213 C214 1.385(12) . ? C213 H213 0.9300 . ? C214 C215 1.382(14) . ? C214 H214 0.9300 . ? C215 C216 1.374(14) . ? C215 H215 0.9300 . ? C216 C217 1.372(11) . ? C216 H216 0.9300 . ? C217 H217 0.9300 . ? C218 C219 1.373(9) . ? C218 C223 1.405(9) . ? C219 C220 1.391(10) . ? C219 H219 0.9300 . ? C220 C221 1.359(11) . ? C220 H220 0.9300 . ? C221 C222 1.387(11) . ? C221 H221 0.9300 . ? C222 C223 1.358(10) . ? C222 H222 0.9300 . ? C223 H223 0.9300 . ? C300 Cl30 1.7027 . ? C300 Cl31 1.7111 . ? C300 H30 1.0163 . ? C300 H31 1.0126 . ? 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 S1 Mo1 S3 108.47(5) . . ? S1 Mo1 S7 108.71(5) . . ? S3 Mo1 S7 84.69(5) . . ? S1 Mo1 S2 86.02(6) . . ? S3 Mo1 S2 49.29(6) . . ? S7 Mo1 S2 133.79(6) . . ? S1 Mo1 S6 84.86(5) . . ? S3 Mo1 S6 133.33(6) . . ? S7 Mo1 S6 49.08(5) . . ? S2 Mo1 S6 170.79(6) . . ? S1 Mo1 Mo2 54.16(4) . . ? S3 Mo1 Mo2 54.63(4) . . ? S7 Mo1 Mo2 96.45(4) . . ? S2 Mo1 Mo2 56.50(4) . . ? S6 Mo1 Mo2 116.33(4) . . ? S1 Mo1 Mo3 54.08(4) . . ? S3 Mo1 Mo3 94.86(4) . . ? S7 Mo1 Mo3 55.16(4) . . ? S2 Mo1 Mo3 116.45(4) . . ? S6 Mo1 Mo3 56.47(4) . . ? Mo2 Mo1 Mo3 59.999(18) . . ? S1 Mo1 I1 80.41(4) . . ? S3 Mo1 I1 135.52(5) . . ? S7 Mo1 I1 135.05(4) . . ? S2 Mo1 I1 89.72(4) . . ? S6 Mo1 I1 90.05(4) . . ? Mo2 Mo1 I1 121.68(2) . . ? Mo3 Mo1 I1 122.47(2) . . ? S1 Mo1 I2 163.42(4) . . ? S3 Mo1 I2 81.73(4) . . ? S7 Mo1 I2 84.79(4) . . ? S2 Mo1 I2 91.44(4) . . ? S6 Mo1 I2 97.68(4) . . ? Mo2 Mo1 I2 135.83(2) . . ? Mo3 Mo1 I2 139.91(2) . . ? I1 Mo1 I2 83.197(19) . . ? S1 Mo2 S3 108.79(6) . . ? S1 Mo2 S5 108.77(5) . . ? S3 Mo2 S5 83.65(6) . . ? S1 Mo2 S4 85.44(5) . . ? S3 Mo2 S4 132.43(6) . . ? S5 Mo2 S4 49.12(5) . . ? S1 Mo2 S2 85.92(6) . . ? S3 Mo2 S2 49.30(6) . . ? S5 Mo2 S2 132.69(6) . . ? S4 Mo2 S2 171.09(6) . . ? S1 Mo2 Mo1 54.21(4) . . ? S3 Mo2 Mo1 54.90(4) . . ? S5 Mo2 Mo1 95.65(4) . . ? S4 Mo2 Mo1 116.26(4) . . ? S2 Mo2 Mo1 56.29(4) . . ? S1 Mo2 Mo3 54.10(4) . . ? S3 Mo2 Mo3 95.04(4) . . ? S5 Mo2 Mo3 55.08(4) . . ? S4 Mo2 Mo3 56.32(4) . . ? S2 Mo2 Mo3 116.25(4) . . ? Mo1 Mo2 Mo3 60.008(18) . . ? S1 Mo2 I3 80.21(4) . . ? S3 Mo2 I3 135.85(5) . . ? S5 Mo2 I3 135.77(4) . . ? S4 Mo2 I3 90.48(4) . . ? S2 Mo2 I3 90.19(4) . . ? Mo1 Mo2 I3 121.76(2) . . ? Mo3 Mo2 I3 122.13(2) . . ? S1 Mo2 I4 162.96(4) . . ? S3 Mo2 I4 83.56(4) . . ? S5 Mo2 I4 83.71(4) . . ? S4 Mo2 I4 94.84(4) . . ? S2 Mo2 I4 94.06(4) . . ? Mo1 Mo2 I4 138.10(2) . . ? Mo3 Mo2 I4 138.54(2) . . ? I3 Mo2 I4 82.745(18) . . ? S1 Mo3 S5 108.65(5) . . ? S1 Mo3 S7 108.63(5) . . ? S5 Mo3 S7 85.32(5) . . ? S1 Mo3 S4 85.59(5) . . ? S5 Mo3 S4 49.10(5) . . ? S7 Mo3 S4 134.15(5) . . ? S1 Mo3 S6 85.01(5) . . ? S5 Mo3 S6 134.01(5) . . ? S7 Mo3 S6 49.05(5) . . ? S4 Mo3 S6 170.54(6) . . ? S1 Mo3 Mo2 54.19(4) . . ? S5 Mo3 Mo2 54.87(4) . . ? S7 Mo3 Mo2 96.29(4) . . ? S4 Mo3 Mo2 56.46(4) . . ? S6 Mo3 Mo2 116.42(4) . . ? S1 Mo3 Mo1 54.23(4) . . ? S5 Mo3 Mo1 95.50(4) . . ? S7 Mo3 Mo1 54.95(4) . . ? S4 Mo3 Mo1 116.38(4) . . ? S6 Mo3 Mo1 56.56(4) . . ? Mo2 Mo3 Mo1 59.993(18) . . ? S1 Mo3 I5 80.73(4) . . ? S5 Mo3 I5 135.31(4) . . ? S7 Mo3 I5 134.37(4) . . ? S4 Mo3 I5 90.09(4) . . ? S6 Mo3 I5 89.40(4) . . ? Mo2 Mo3 I5 122.40(2) . . ? Mo1 Mo3 I5 122.45(2) . . ? S1 Mo3 I6 161.80(4) . . ? S5 Mo3 I6 83.40(4) . . ? S7 Mo3 I6 85.42(4) . . ? S4 Mo3 I6 92.82(4) . . ? S6 Mo3 I6 96.43(4) . . ? Mo2 Mo3 I6 137.75(2) . . ? Mo1 Mo3 I6 140.20(2) . . ? I5 Mo3 I6 81.144(18) . . ? Mo3 S1 Mo2 71.71(4) . . ? Mo3 S1 Mo1 71.69(4) . . ? Mo2 S1 Mo1 71.63(4) . . ? S3 S2 Mo1 62.94(6) . . ? S3 S2 Mo2 62.58(6) . . ? Mo1 S2 Mo2 67.21(4) . . ? S2 S3 Mo2 68.12(7) . . ? S2 S3 Mo1 67.77(7) . . ? Mo2 S3 Mo1 70.47(4) . . ? S5 S4 Mo3 63.32(6) . . ? S5 S4 Mo2 63.05(6) . . ? Mo3 S4 Mo2 67.22(4) . . ? S4 S5 Mo2 67.84(6) . . ? S4 S5 Mo3 67.58(6) . . ? Mo2 S5 Mo3 70.05(4) . . ? S7 S6 Mo3 63.25(6) . . ? S7 S6 Mo1 63.00(6) . . ? Mo3 S6 Mo1 66.98(4) . . ? S6 S7 Mo1 67.92(6) . . ? S6 S7 Mo3 67.70(6) . . ? Mo1 S7 Mo3 69.89(4) . . ? C112 P100 C106 110.1(4) . . ? C112 P100 C118 108.8(4) . . ? C106 P100 C118 109.1(4) . . ? C112 P100 C100 108.4(4) . . ? C106 P100 C100 108.7(4) . . ? C118 P100 C100 111.7(4) . . ? C206 P200 C200 107.2(3) . . ? C206 P200 C212 109.3(3) . . ? C200 P200 C212 112.6(3) . . ? C206 P200 C218 111.5(3) . . ? C200 P200 C218 109.4(3) . . ? C212 P200 C218 106.9(3) . . ? C105 C100 C101 119.6(9) . . ? C105 C100 P100 120.3(7) . . ? C101 C100 P100 120.0(8) . . ? C102 C101 C100 118.7(11) . . ? C102 C101 H101 120.7 . . ? C100 C101 H101 120.7 . . ? C103 C102 C101 120.8(11) . . ? C103 C102 H102 119.6 . . ? C101 C102 H102 119.6 . . ? C104 C103 C102 120.7(10) . . ? C104 C103 H103 119.7 . . ? C102 C103 H103 119.7 . . ? C103 C104 C105 120.7(11) . . ? C103 C104 H104 119.6 . . ? C105 C104 H104 119.6 . . ? C104 C105 C100 119.5(10) . . ? C104 C105 H105 120.2 . . ? C100 C105 H105 120.2 . . ? C107 C106 C111 119.7(8) . . ? C107 C106 P100 119.3(7) . . ? C111 C106 P100 120.7(6) . . ? C106 C107 C108 120.8(10) . . ? C106 C107 H107 119.6 . . ? C108 C107 H107 119.6 . . ? C109 C108 C107 118.7(10) . . ? C109 C108 H108 120.7 . . ? C107 C108 H108 120.7 . . ? C110 C109 C108 120.2(9) . . ? C110 C109 H109 119.9 . . ? C108 C109 H109 119.9 . . ? C109 C110 C111 118.3(9) . . ? C109 C110 H110 120.8 . . ? C111 C110 H110 120.8 . . ? C110 C111 C106 121.8(9) . . ? C110 C111 H111 119.1 . . ? C106 C111 H111 119.1 . . ? C113 C112 C117 119.5(8) . . ? C113 C112 P100 121.1(7) . . ? C117 C112 P100 119.3(7) . . ? C112 C113 C114 119.6(9) . . ? C112 C113 H113 120.2 . . ? C114 C113 H113 120.2 . . ? C115 C114 C113 119.8(9) . . ? C115 C114 H114 120.1 . . ? C113 C114 H114 120.1 . . ? C114 C115 C116 121.3(9) . . ? C114 C115 H115 119.4 . . ? C116 C115 H115 119.4 . . ? C117 C116 C115 118.5(9) . . ? C117 C116 H116 120.8 . . ? C115 C116 H116 120.8 . . ? C116 C117 C112 121.3(9) . . ? C116 C117 H117 119.3 . . ? C112 C117 H117 119.3 . . ? C123 C118 C119 119.4(9) . . ? C123 C118 P100 121.1(8) . . ? C119 C118 P100 119.5(7) . . ? C120 C119 C118 120.0(9) . . ? C120 C119 H119 120.0 . . ? C118 C119 H119 120.0 . . ? C121 C120 C119 121.3(10) . . ? C121 C120 H120 119.4 . . ? C119 C120 H120 119.4 . . ? C120 C121 C122 118.8(11) . . ? C120 C121 H121 120.6 . . ? C122 C121 H121 120.6 . . ? C121 C122 C123 121.0(12) . . ? C121 C122 H122 119.5 . . ? C123 C122 H122 119.5 . . ? C118 C123 C122 119.4(11) . . ? C118 C123 H123 120.3 . . ? C122 C123 H123 120.3 . . ? C205 C200 C201 118.8(6) . . ? C205 C200 P200 120.6(5) . . ? C201 C200 P200 120.5(5) . . ? C202 C201 C200 119.6(7) . . ? C202 C201 H201 120.2 . . ? C200 C201 H201 120.2 . . ? C203 C202 C201 120.6(8) . . ? C203 C202 H202 119.7 . . ? C201 C202 H202 119.7 . . ? C204 C203 C202 119.8(7) . . ? C204 C203 H203 120.1 . . ? C202 C203 H203 120.1 . . ? C203 C204 C205 120.7(7) . . ? C203 C204 H204 119.6 . . ? C205 C204 H204 119.6 . . ? C200 C205 C204 120.5(7) . . ? C200 C205 H205 119.8 . . ? C204 C205 H205 119.8 . . ? C211 C206 C207 121.0(7) . . ? C211 C206 P200 120.3(6) . . ? C207 C206 P200 118.4(6) . . ? C206 C207 C208 117.7(9) . . ? C206 C207 H207 121.2 . . ? C208 C207 H207 121.2 . . ? C209 C208 C207 120.9(9) . . ? C209 C208 H208 119.5 . . ? C207 C208 H208 119.5 . . ? C208 C209 C210 120.8(8) . . ? C208 C209 H209 119.6 . . ? C210 C209 H209 119.6 . . ? C209 C210 C211 119.2(10) . . ? C209 C210 H210 120.4 . . ? C211 C210 H210 120.4 . . ? C206 C211 C210 120.4(9) . . ? C206 C211 H211 119.8 . . ? C210 C211 H211 119.8 . . ? C217 C212 C213 120.1(7) . . ? C217 C212 P200 119.3(6) . . ? C213 C212 P200 120.2(5) . . ? C214 C213 C212 119.4(8) . . ? C214 C213 H213 120.3 . . ? C212 C213 H213 120.3 . . ? C215 C214 C213 119.8(9) . . ? C215 C214 H214 120.1 . . ? C213 C214 H214 120.1 . . ? C216 C215 C214 120.6(8) . . ? C216 C215 H215 119.7 . . ? C214 C215 H215 119.7 . . ? C217 C216 C215 120.0(9) . . ? C217 C216 H216 120.0 . . ? C215 C216 H216 120.0 . . ? C216 C217 C212 120.1(8) . . ? C216 C217 H217 119.9 . . ? C212 C217 H217 119.9 . . ? C219 C218 C223 120.3(6) . . ? C219 C218 P200 120.0(5) . . ? C223 C218 P200 119.6(5) . . ? C218 C219 C220 119.5(7) . . ? C218 C219 H219 120.3 . . ? C220 C219 H219 120.3 . . ? C221 C220 C219 120.3(7) . . ? C221 C220 H220 119.9 . . ? C219 C220 H220 119.9 . . ? C220 C221 C222 120.0(7) . . ? C220 C221 H221 120.0 . . ? C222 C221 H221 120.0 . . ? C223 C222 C221 121.1(7) . . ? C223 C222 H222 119.5 . . ? C221 C222 H222 119.5 . . ? C222 C223 C218 118.8(7) . . ? C222 C223 H223 120.6 . . ? C218 C223 H223 120.6 . . ? Cl30 C300 Cl31 118.1 . . ? Cl30 C300 H30 108.5 . . ? Cl31 C300 H30 110.5 . . ? Cl30 C300 H31 108.3 . . ? Cl31 C300 H31 106.9 . . ? H30 C300 H31 103.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.493 _refine_diff_density_min -1.099 _refine_diff_density_rms 0.246 #===END data_(PPh4)3[2] _database_code_depnum_ccdc_archive 'CCDC 713964' # start Validation Reply Form _vrf_PLAT083_compound2 ; PROBLEM: SHELXL Second Parameter in WGHT unusually Large. 71.00 RESPONSE: See Supplementary Materials for a full text description of the solution and refinement of the structure of (PPh4)3[2].2Me2C=O. With respect to this alert, as described in the supplementary text, the diffracted intensity dropped off sharply at 2-theta values corresponding to about 1 A resolution. This necessarily gave a non-normal distribution of errors in the data, which is one of the two generally accepted possible causes of the need for a large second parameter in the SHELXL-97 weighting scheme. The other possible cause of this effect, the presence of twinning (or some other systematic feature of the crystal that perturbs the distribution of intensities and/or their errors) was tested thoroughly, and no direct evidence for twinning emerged. Except for the unusual distribution of intensities, none of the usual symptoms of twinning is present. In addition, the clear presence of ordered chemical residues on sites of crystallographic symmetry (-4) and (23) in space group P(-4)3n, Laue class m(-3)m, effectively rules out merohedral twinning. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H72 I19 Mo12 O2 P3 S28' _chemical_formula_weight 5594.33 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' I I -0.4742 1.8119 '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' P P 0.1023 0.0942 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M 'P -4 3 n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y+1/2, -x+1/2, -z+1/2' '-x, -y, z' '-y+1/2, x+1/2, -z+1/2' 'x, -y, -z' '-y+1/2, -x+1/2, z+1/2' '-x, y, -z' 'y+1/2, x+1/2, z+1/2' 'z, x, y' 'x+1/2, -z+1/2, -y+1/2' '-z, -x, y' '-x+1/2, z+1/2, -y+1/2' 'z, -x, -y' '-x+1/2, -z+1/2, y+1/2' '-z, x, -y' 'x+1/2, z+1/2, y+1/2' 'y, z, x' 'z+1/2, y+1/2, x+1/2' 'z+1/2, -y+1/2, -x+1/2' '-z+1/2, -y+1/2, x+1/2' '-z+1/2, y+1/2, -x+1/2' 'y, -z, -x' '-y, -z, x' '-y, z, -x' _cell_length_a 19.086(4) _cell_length_b 19.086(4) _cell_length_c 19.086(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6953(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7919 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 28.79 _exptl_crystal_description irregular _exptl_crystal_colour red _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5120 _exptl_absorpt_coefficient_mu 5.753 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7327 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details 'SADABS (Bruker, 2002)' _exptl_special_details ; The crystal had a frond-like morphology with re-entrant faces. This obviates the use of a morphology-based absorption correction. In addition, because of this suggestive morphology a complete battery of tests and alternative structural models was used to check for twinning. ; _diffrn_ambient_temperature 100(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 'D8 Apex' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean 85.3 _diffrn_reflns_number 51071 _diffrn_reflns_av_R_equivalents 0.0808 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 4.27 _diffrn_reflns_theta_max 25.99 _reflns_number_total 2278 _reflns_number_gt 1760 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART V5.624 (Bruker, 2001)' _computing_cell_refinement 'SAINT V6.02A (Bruker, 2000)' _computing_data_reduction 'SAINT V6.02A (Bruker, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond (Brandenburg, 2007)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Four dummy atoms -- symmetry relatives of C8 and O1Z with zero occupancy, were used in the refinement as geometrical placeholders for the application of restraints to the solvent acetone disorder assembly. 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^)+(0.0497P)^2^+70.9584P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'refinement of absolute structure parameter (Flack, 1983)' _refine_ls_abs_structure_Flack 0.05(6) _refine_ls_number_reflns 2278 _refine_ls_number_parameters 124 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0532 _refine_ls_wR_factor_ref 0.1275 _refine_ls_wR_factor_gt 0.1195 _refine_ls_goodness_of_fit_ref 1.158 _refine_ls_restrained_S_all 1.144 _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 Mo1 Mo 0.40213(7) 0.40414(7) 0.30174(6) 0.0361(3) Uani 1 1 d . . . I1 I 0.5000 0.5000 0.23434(6) 0.0403(3) Uani 1 2 d S . . I2 I 0.37356(5) 0.37984(5) 0.16082(5) 0.0405(2) Uani 1 1 d . . . I3 I 0.5000 0.5000 0.5000 0.0428(7) Uani 1 12 d S . . S1 S 0.49930(18) 0.37914(19) 0.37689(19) 0.0395(7) Uani 1 1 d . . . S2 S 0.48754(18) 0.3059(2) 0.3019(2) 0.0395(8) Uani 1 1 d . . . S3 S 0.31662(17) 0.31662(17) 0.31662(17) 0.0357(12) Uani 1 3 d S . . P1 P 0.0000 0.5000 0.2500 0.0372(16) Uani 1 4 d S . . C1 C 0.0716(9) 0.4758(9) 0.1932(9) 0.052(4) Uani 1 1 d . . . C2 C 0.1401(8) 0.4968(8) 0.2094(9) 0.048(4) Uani 1 1 d . . . H2 H 0.1500 0.5224 0.2509 0.058 Uiso 1 1 calc R . . C3 C 0.1918(9) 0.4794(9) 0.1637(10) 0.051(4) Uani 1 1 d . . . H3 H 0.2383 0.4944 0.1730 0.061 Uiso 1 1 calc R . . C4 C 0.1790(10) 0.4407(9) 0.1046(10) 0.059(5) Uani 1 1 d . . . H4 H 0.2167 0.4254 0.0759 0.071 Uiso 1 1 calc R . . C5 C 0.1128(12) 0.4249(11) 0.0876(11) 0.079(7) Uani 1 1 d . . . H5 H 0.1032 0.4029 0.0440 0.095 Uiso 1 1 calc R . . C6 C 0.0593(10) 0.4396(10) 0.1320(10) 0.059(5) Uani 1 1 d . . . H6 H 0.0131 0.4250 0.1208 0.071 Uiso 1 1 calc R . . C7 C 0.2058(12) 0.2058(12) 0.2058(12) 0.028(4) Uani 0.25 3 d SPDU . . O1 O 0.1560(12) 0.1560(12) 0.1560(12) 0.026(5) Uani 0.25 3 d SPDU . . C8 C 0.178(2) 0.2741(10) 0.1762(18) 0.028(4) Uani 0.3333 1 d PDU . . O1Z O 0.171(5) 0.253(3) 0.182(3) 0.028(4) Uani 0.0833 1 d PDU . . C7Z C 0.1992(15) 0.1984(14) 0.1696(14) 0.028(4) Uani 0.0833 1 d PDU . . 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 Mo1 0.0362(7) 0.0351(7) 0.0371(6) -0.0021(6) -0.0014(6) -0.0035(5) I1 0.0427(8) 0.0436(8) 0.0346(6) 0.000 0.000 -0.0097(6) I2 0.0403(6) 0.0450(6) 0.0361(5) -0.0042(4) -0.0006(4) -0.0027(4) I3 0.0428(7) 0.0428(7) 0.0428(7) 0.000 0.000 0.000 S1 0.0366(16) 0.042(2) 0.040(2) -0.0017(14) -0.0026(16) -0.0006(16) S2 0.0378(19) 0.040(2) 0.041(2) -0.0030(14) 0.0014(16) -0.0035(16) S3 0.0357(12) 0.0357(12) 0.0357(12) -0.0033(13) -0.0033(13) -0.0033(13) P1 0.035(2) 0.035(2) 0.041(4) 0.000 0.000 0.000 C1 0.048(10) 0.052(10) 0.057(11) 0.008(8) 0.010(8) 0.003(8) C2 0.051(10) 0.031(8) 0.062(10) 0.001(8) -0.006(8) 0.015(8) C3 0.043(9) 0.051(10) 0.059(10) 0.002(8) 0.008(8) 0.003(8) C4 0.051(11) 0.056(10) 0.070(13) -0.020(9) 0.033(9) -0.011(9) C5 0.103(17) 0.075(13) 0.060(12) -0.033(10) 0.038(13) -0.029(12) C6 0.048(10) 0.066(12) 0.062(12) -0.026(10) 0.006(9) -0.014(8) C7 0.028(4) 0.028(4) 0.028(4) 0.007(4) 0.007(4) 0.007(4) O1 0.026(5) 0.026(5) 0.026(5) 0.006(5) 0.006(5) 0.006(5) C8 0.029(5) 0.026(5) 0.029(5) 0.008(5) 0.008(5) 0.005(5) O1Z 0.029(5) 0.026(5) 0.029(5) 0.008(5) 0.008(5) 0.005(5) C7Z 0.028(4) 0.028(4) 0.028(4) 0.007(4) 0.007(4) 0.007(4) _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 S3 2.353(4) . ? Mo1 S1 2.390(4) 9 ? Mo1 S1 2.393(4) . ? Mo1 S2 2.484(4) . ? Mo1 S2 2.490(4) 9 ? Mo1 Mo1 2.737(2) 17 ? Mo1 Mo1 2.737(2) 9 ? Mo1 I2 2.7831(16) . ? Mo1 I1 2.9140(14) . ? I1 Mo1 2.9140(14) 3_665 ? S1 S2 2.013(5) . ? S1 Mo1 2.390(4) 17 ? S2 Mo1 2.490(4) 17 ? S3 Mo1 2.353(4) 17 ? S3 Mo1 2.353(4) 9 ? P1 C1 1.804(17) . ? C1 C6 1.38(3) . ? C1 C2 1.40(2) . ? C2 C3 1.36(2) . ? C2 H2 0.9500 . ? C3 C4 1.37(2) . ? C3 H3 0.9500 . ? C4 C5 1.34(3) . ? C4 H4 0.9500 . ? C5 C6 1.36(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O1Z 1.22(2) . ? C7 C8 1.517(16) . ? O1 C7Z 1.18(2) . ? C8 C7Z 1.507(19) . ? C7Z C8 1.499(19) 17 ? 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 S3 Mo1 S1 108.97(12) . 9 ? S3 Mo1 S1 108.89(12) . . ? S1 Mo1 S1 86.41(17) 9 . ? S3 Mo1 S2 85.37(9) . . ? S1 Mo1 S2 134.84(13) 9 . ? S1 Mo1 S2 48.72(12) . . ? S3 Mo1 S2 85.23(10) . 9 ? S1 Mo1 S2 48.67(12) 9 9 ? S1 Mo1 S2 134.74(13) . 9 ? S2 Mo1 S2 170.57(14) . 9 ? S3 Mo1 Mo1 54.43(8) . 17 ? S1 Mo1 Mo1 96.47(9) 9 17 ? S1 Mo1 Mo1 55.04(10) . 17 ? S2 Mo1 Mo1 56.72(11) . 17 ? S2 Mo1 Mo1 116.40(11) 9 17 ? S3 Mo1 Mo1 54.43(7) . 9 ? S1 Mo1 Mo1 55.13(10) 9 9 ? S1 Mo1 Mo1 96.41(9) . 9 ? S2 Mo1 Mo1 116.62(11) . 9 ? S2 Mo1 Mo1 56.51(11) 9 9 ? Mo1 Mo1 Mo1 60.0 17 9 ? S3 Mo1 I2 82.09(10) . . ? S1 Mo1 I2 133.19(10) 9 . ? S1 Mo1 I2 134.26(10) . . ? S2 Mo1 I2 90.21(10) . . ? S2 Mo1 I2 89.25(10) 9 . ? Mo1 Mo1 I2 124.07(5) 17 . ? Mo1 Mo1 I2 123.40(5) 9 . ? S3 Mo1 I1 160.70(11) . . ? S1 Mo1 I1 85.70(10) 9 . ? S1 Mo1 I1 83.86(10) . . ? S2 Mo1 I1 93.07(10) . . ? S2 Mo1 I1 96.05(10) 9 . ? Mo1 Mo1 I1 138.44(6) 17 . ? Mo1 Mo1 I1 140.60(6) 9 . ? I2 Mo1 I1 78.67(4) . . ? Mo1 I1 Mo1 127.61(6) 3_665 . ? S2 S1 Mo1 68.27(15) . 17 ? S2 S1 Mo1 68.02(15) . . ? Mo1 S1 Mo1 69.83(10) 17 . ? S1 S2 Mo1 63.26(15) . . ? S1 S2 Mo1 63.06(15) . 17 ? Mo1 S2 Mo1 66.77(11) . 17 ? Mo1 S3 Mo1 71.14(15) . 17 ? Mo1 S3 Mo1 71.14(15) . 9 ? Mo1 S3 Mo1 71.14(15) 17 9 ? C1 P1 C1 111.2(6) . 4 ? C1 P1 C1 106.1(12) . 3_565 ? C1 P1 C1 111.2(6) 4 3_565 ? C1 P1 C1 111.2(6) . 2_455 ? C1 P1 C1 106.1(12) 4 2_455 ? C1 P1 C1 111.2(6) 3_565 2_455 ? C6 C1 C2 119.3(16) . . ? C6 C1 P1 120.6(14) . . ? C2 C1 P1 120.0(14) . . ? C3 C2 C1 117.8(17) . . ? C3 C2 H2 121.1 . . ? C1 C2 H2 121.1 . . ? C2 C3 C4 122.0(16) . . ? C2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? C5 C4 C3 119.3(16) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 120.8(19) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 120.4(18) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? O1Z C7 C8 113(5) . 9 ? O1Z C7 C8 128(5) . 17 ? C8 C7 C8 119.4(4) 9 17 ? O1 C7Z C8 119.1(17) . . ? O1 C7Z C8 119.7(18) . 17 ? C8 C7Z C8 121(3) 17 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 P1 C1 C6 -159.0(16) 4 . . . ? C1 P1 C1 C6 -38.0(13) 3_565 . . . ? C1 P1 C1 C6 83.0(12) 2_455 . . . ? C1 P1 C1 C2 17.8(15) 4 . . . ? C1 P1 C1 C2 138.8(16) 3_565 . . . ? C1 P1 C1 C2 -100.1(18) 2_455 . . . ? C6 C1 C2 C3 -1(2) . . . . ? P1 C1 C2 C3 -177.7(12) . . . . ? C1 C2 C3 C4 -2(2) . . . . ? C2 C3 C4 C5 6(3) . . . . ? C3 C4 C5 C6 -7(3) . . . . ? C4 C5 C6 C1 5(3) . . . . ? C2 C1 C6 C5 0(3) . . . . ? P1 C1 C6 C5 176.5(16) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.401 _refine_diff_density_min -0.903 _refine_diff_density_rms 0.170