Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_p46ka _database_code_CSD 180468 _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Szczepura, Lisa' 'Ooro, Betty A.' 'Wilson, Scott' _publ_contact_author_name 'Prof Lisa Szczepura' _publ_contact_author_address ; Chemistry Harvard University Chemical Laboratories #147 12 Oxford Street Cambridge MA 02138 UNITED STATES OF AMERICA ; _publ_contact_author_phone '1 309 438-2359 ' _publ_contact_author_fax '1 309 438-5538 ' _publ_contact_author_email 'SZCZEPURA@RADCLIFFE.RIASPO' _publ_section_title ; Synthesis of Hexanuclear Molybdenum Clusters Containing Phosphine Oxide Ligands ; _publ_section_references ; Sheldrick, G.M. (1998). SHELX-97-2. Program for crystal structure solution and refinement. Institute fur anorg chemie, Gottingen, Germany. Bruker AXS, Inc. (1998). Madison, Wisconsin, USA. ; _publ_section_figure_captions ; Figure 1. SHELXTL (Bruker, 1998) plot showing 35% probability ellipsoids for non-H atoms and circles of arbitrary size for H atoms. ; _publ_section_exptl_prep ; Crystals were grown from chloroform. ; _publ_section_exptl_refinement ; Systematic conditions suggested the unambiguous space group. Structure was solved by direct methods (Sheldrick, 1998). Proposed model describes all propyl moieties occupying two disordered sites. Inversion symmetry was imposed on the host comnplex. Propyl groups were idealized using pseudo-threefold symmetry (effective standard deviation 0.02 \%A), equivalent C-C bond lengths and angles (esd 0.01 \%A). Rigid bond restraints (esd 0.01) were applied to disordered positions separated by less than 1.5 \%A. Displacement parameters for disorder positions were further restrained to be similar (esd 0.04). H atoms were included as riding idealized contributors. H atom U's were assigned as 1.2 times Ueq of adjacent non-H atoms. The space group choice was confirmed by successful convergence of the full-matrix least-squares refinement on F^2^ (Sheldrick, 1998). The highest peak in the final difference Fourier map was in the vicinity of atom Cl7; the final map had no other significant features. A final analysis of variance between observed and calculated structure factors showed no dependence on amplitude or resolution. ; _audit_creation_method SHELXL-97 _audit_update_record ; ? ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H42 Cl12 Mo6 O2 P2, 2(C H Cl3)' _chemical_formula_sum 'C20 H44 Cl18 Mo6 O2 P2' _chemical_formula_structural ? _chemical_formula_weight 1592.23 _chemical_formula_analytical ? _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' 'P' 'P' 0.1023 0.0942 '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_H-M 'P21/n ' _symmetry_space_group_name_Hall '-P 2yn ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.0685(16) _cell_length_b 15.617(2) _cell_length_c 15.693(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.799(5) _cell_angle_gamma 90.00 _cell_volume 2466.3(7) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 923 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 27.8 _exptl_crystal_description 'tabular' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.144 _exptl_crystal_density_method ? _exptl_crystal_F_000 1536 _exptl_crystal_preparation ; The data crystal was mounted using oil (Parantone-N, Exxon) to a thin glass fiber with the (0 1 -1) scattering planes roughly normal to the spindle axis. ; _exptl_crystal_id p46ka _exptl_absorpt_coefficient_mu 2.542 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_correction_T_min 0.5564 _exptl_absorpt_correction_T_max 0.8692 _exptl_absorpt_process_details '(Bruker, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id p46ka _diffrn_radiation_type 'MoK\a' _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type ? _diffrn_measurement_device 'Siemens Platform/CCD' _diffrn_measurement_method 'profile data from \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 341 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 552 _diffrn_standards_decay_% 0.5 _diffrn_reflns_number 18342 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0415 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.31 _reflns_number_total 4492 _reflns_number_gt 3341 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART V5 (Bruker, 1998)' _computing_cell_refinement 'SAINT V5 (Bruker, 1998)' _computing_data_reduction 'SAINT V5 (Bruker, 1998)' _computing_structure_solution 'SHELXTL V5 (Bruker, 1998)' _computing_structure_refinement 'SHELXTL V5 (Bruker, 1998)' _computing_molecular_graphics 'SHELXTL V5 (Bruker, 1998)' _computing_publication_material 'CIFTAB (Sheldrick, 1998)' _refine_special_details ; ? ; _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^)+(0.0320P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4492 _refine_ls_number_parameters 299 _refine_ls_number_restraints 293 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0288 _refine_ls_wR_factor_ref 0.0672 _refine_ls_wR_factor_gt 0.0626 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _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 0.10014(4) 0.09043(2) 0.54015(2) 0.02906(11) Uani 1 1 d . . . Mo2 Mo -0.04915(4) -0.02430(2) 0.60941(2) 0.02945(11) Uani 1 1 d . . . Mo3 Mo 0.14482(4) -0.07119(2) 0.51402(2) 0.02918(11) Uani 1 1 d . . . Cl1 Cl 0.27964(10) 0.04159(7) 0.44799(7) 0.0388(3) Uani 1 1 d . . . Cl2 Cl 0.00514(11) 0.17728(6) 0.42146(6) 0.0374(3) Uani 1 1 d . . . Cl3 Cl -0.08867(11) 0.13082(7) 0.62847(6) 0.0400(3) Uani 1 1 d . . . Cl4 Cl 0.18644(11) -0.00421(7) 0.65501(6) 0.0405(3) Uani 1 1 d . . . Cl5 Cl -0.10910(13) -0.05608(8) 0.75351(7) 0.0560(4) Uani 1 1 d . . . Cl6 Cl 0.33388(12) -0.16564(8) 0.53472(8) 0.0531(3) Uani 1 1 d . . . P1 P 0.28447(12) 0.27213(7) 0.61288(8) 0.0416(3) Uani 1 1 d D . . O1 O 0.2149(3) 0.1914(2) 0.5879(2) 0.0552(9) Uani 1 1 d . A . C1 C 0.2036(7) 0.3305(6) 0.6944(5) 0.061(3) Uani 0.540(5) 1 d PDU A 1 H1A H 0.2099 0.2964 0.7475 0.073 Uiso 0.540(5) 1 calc PR A 1 H1B H 0.2537 0.3842 0.7048 0.073 Uiso 0.540(5) 1 calc PR A 1 C2 C 0.0585(8) 0.3536(7) 0.6775(6) 0.065(3) Uani 0.540(5) 1 d PDU A 1 H2A H 0.0511 0.3887 0.6250 0.078 Uiso 0.540(5) 1 calc PR A 1 H2B H 0.0072 0.3003 0.6671 0.078 Uiso 0.540(5) 1 calc PR A 1 C3 C -0.0020(10) 0.4018(9) 0.7492(8) 0.076(4) Uani 0.540(5) 1 d PDU A 1 H3A H 0.0652 0.4391 0.7764 0.091 Uiso 0.540(5) 1 calc PR A 1 H3B H -0.0347 0.3612 0.7913 0.091 Uiso 0.540(5) 1 calc PR A 1 H3C H -0.0761 0.4367 0.7269 0.091 Uiso 0.540(5) 1 calc PR A 1 C4 C 0.2836(10) 0.3397(6) 0.5192(4) 0.069(3) Uani 0.540(5) 1 d PDU A 1 H4A H 0.1917 0.3602 0.5077 0.083 Uiso 0.540(5) 1 calc PR A 1 H4B H 0.3397 0.3905 0.5317 0.083 Uiso 0.540(5) 1 calc PR A 1 C5 C 0.3329(13) 0.2970(6) 0.4384(5) 0.064(3) Uani 0.540(5) 1 d PDU A 1 H5A H 0.4264 0.2790 0.4482 0.077 Uiso 0.540(5) 1 calc PR A 1 H5B H 0.2794 0.2449 0.4264 0.077 Uiso 0.540(5) 1 calc PR A 1 C6 C 0.3240(16) 0.3547(8) 0.3629(5) 0.109(4) Uani 0.540(5) 1 d PDU A 1 H6A H 0.3757 0.4067 0.3747 0.130 Uiso 0.540(5) 1 calc PR A 1 H6B H 0.2309 0.3699 0.3509 0.130 Uiso 0.540(5) 1 calc PR A 1 H6C H 0.3597 0.3253 0.3134 0.130 Uiso 0.540(5) 1 calc PR A 1 C7 C 0.4509(6) 0.2509(6) 0.6439(5) 0.058(2) Uani 0.540(5) 1 d PDU A 1 H7A H 0.5011 0.2335 0.5935 0.070 Uiso 0.540(5) 1 calc PR A 1 H7B H 0.4924 0.3034 0.6680 0.070 Uiso 0.540(5) 1 calc PR A 1 C8 C 0.4570(9) 0.1798(8) 0.7101(8) 0.083(3) Uani 0.540(5) 1 d PDU A 1 H8A H 0.4147 0.2004 0.7624 0.100 Uiso 0.540(5) 1 calc PR A 1 H8B H 0.4043 0.1305 0.6882 0.100 Uiso 0.540(5) 1 calc PR A 1 C9 C 0.5929(10) 0.1497(8) 0.7331(8) 0.102(4) Uani 0.540(5) 1 d PDU A 1 H9A H 0.6455 0.1976 0.7564 0.122 Uiso 0.540(5) 1 calc PR A 1 H9B H 0.6349 0.1274 0.6822 0.122 Uiso 0.540(5) 1 calc PR A 1 H9C H 0.5883 0.1043 0.7760 0.122 Uiso 0.540(5) 1 calc PR A 1 C10 C 0.1609(9) 0.3461(7) 0.6459(6) 0.066(3) Uani 0.460(5) 1 d PDU A 2 H10A H 0.2025 0.4029 0.6553 0.079 Uiso 0.460(5) 1 calc PR A 2 H10B H 0.0921 0.3521 0.5999 0.079 Uiso 0.460(5) 1 calc PR A 2 C11 C 0.0948(11) 0.3178(8) 0.7277(7) 0.065(3) Uani 0.460(5) 1 d PDU A 2 H11A H 0.0778 0.2554 0.7248 0.078 Uiso 0.460(5) 1 calc PR A 2 H11B H 0.1567 0.3285 0.7768 0.078 Uiso 0.460(5) 1 calc PR A 2 C12 C -0.0328(12) 0.3629(10) 0.7426(11) 0.086(4) Uani 0.460(5) 1 d PDU A 2 H12A H -0.1055 0.3332 0.7119 0.103 Uiso 0.460(5) 1 calc PR A 2 H12B H -0.0272 0.4219 0.7219 0.103 Uiso 0.460(5) 1 calc PR A 2 H12C H -0.0497 0.3632 0.8037 0.103 Uiso 0.460(5) 1 calc PR A 2 C13 C 0.3847(9) 0.3222(8) 0.5343(6) 0.081(4) Uani 0.460(5) 1 d PDU A 2 H13A H 0.4214 0.3765 0.5576 0.097 Uiso 0.460(5) 1 calc PR A 2 H13B H 0.4602 0.2842 0.5215 0.097 Uiso 0.460(5) 1 calc PR A 2 C14 C 0.3053(17) 0.3407(12) 0.4527(8) 0.110(4) Uani 0.460(5) 1 d PDU A 2 H14A H 0.2129 0.3209 0.4597 0.132 Uiso 0.460(5) 1 calc PR A 2 H14B H 0.3026 0.4034 0.4438 0.132 Uiso 0.460(5) 1 calc PR A 2 C15 C 0.358(2) 0.3000(13) 0.3761(7) 0.143(5) Uani 0.460(5) 1 d PDU A 2 H15A H 0.3312 0.3334 0.3255 0.171 Uiso 0.460(5) 1 calc PR A 2 H15B H 0.3229 0.2417 0.3706 0.171 Uiso 0.460(5) 1 calc PR A 2 H15C H 0.4553 0.2979 0.3811 0.171 Uiso 0.460(5) 1 calc PR A 2 C16 C 0.3957(9) 0.2549(7) 0.7049(5) 0.073(3) Uani 0.460(5) 1 d PDU A 2 H16A H 0.4135 0.3117 0.7309 0.087 Uiso 0.460(5) 1 calc PR A 2 H16B H 0.3458 0.2214 0.7469 0.087 Uiso 0.460(5) 1 calc PR A 2 C17 C 0.5292(9) 0.2111(7) 0.6958(10) 0.080(3) Uani 0.460(5) 1 d PDU A 2 H17A H 0.5777 0.2392 0.6496 0.096 Uiso 0.460(5) 1 calc PR A 2 H17B H 0.5826 0.2182 0.7495 0.096 Uiso 0.460(5) 1 calc PR A 2 C18 C 0.5158(10) 0.1183(6) 0.6766(7) 0.058(3) Uani 0.460(5) 1 d PDU A 2 H18A H 0.4841 0.1109 0.6173 0.069 Uiso 0.460(5) 1 calc PR A 2 H18B H 0.4521 0.0925 0.7149 0.069 Uiso 0.460(5) 1 calc PR A 2 H18C H 0.6024 0.0904 0.6847 0.069 Uiso 0.460(5) 1 calc PR A 2 Cl7 Cl 0.2792(2) -0.41063(12) 0.45295(10) 0.1053(6) Uani 1 1 d . . . Cl8 Cl 0.0690(2) -0.41036(12) 0.57007(14) 0.1062(6) Uani 1 1 d . . . Cl9 Cl 0.3372(2) -0.42613(13) 0.63256(11) 0.1113(7) Uani 1 1 d . . . C19 C 0.2326(6) -0.3808(4) 0.5541(3) 0.0717(17) Uani 1 1 d . . . H19 H 0.2391 -0.3170 0.5587 0.086 Uiso 1 1 calc R . . 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 0.0335(2) 0.0239(2) 0.02974(19) -0.00266(14) -0.00044(16) -0.00320(16) Mo2 0.0362(2) 0.0275(2) 0.02480(18) 0.00018(14) 0.00272(15) -0.00061(16) Mo3 0.0306(2) 0.0245(2) 0.0324(2) 0.00055(14) 0.00094(16) 0.00212(16) Cl1 0.0323(6) 0.0365(6) 0.0481(6) 0.0016(5) 0.0074(5) -0.0028(5) Cl2 0.0432(7) 0.0272(6) 0.0419(6) 0.0070(4) 0.0013(5) 0.0000(5) Cl3 0.0503(7) 0.0325(6) 0.0378(6) -0.0100(4) 0.0086(5) 0.0017(5) Cl4 0.0430(7) 0.0436(7) 0.0343(6) 0.0010(5) -0.0105(5) -0.0018(5) Cl5 0.0722(9) 0.0625(8) 0.0341(6) 0.0087(5) 0.0146(6) -0.0009(7) Cl6 0.0438(7) 0.0423(7) 0.0731(8) 0.0052(6) 0.0012(6) 0.0152(6) P1 0.0425(7) 0.0337(7) 0.0487(7) -0.0100(5) 0.0009(6) -0.0084(6) O1 0.062(2) 0.040(2) 0.062(2) -0.0146(16) -0.0089(17) -0.0199(17) C1 0.044(5) 0.068(6) 0.071(7) -0.027(6) -0.003(5) -0.006(5) C2 0.055(6) 0.065(7) 0.075(6) -0.024(5) 0.002(5) 0.002(5) C3 0.049(6) 0.089(9) 0.090(7) -0.043(7) -0.001(6) 0.008(6) C4 0.082(7) 0.065(6) 0.062(6) 0.003(5) 0.019(6) -0.009(6) C5 0.079(6) 0.068(7) 0.048(5) 0.013(5) 0.032(5) -0.001(6) C6 0.153(9) 0.093(9) 0.082(6) 0.042(6) 0.046(7) 0.045(8) C7 0.044(6) 0.079(6) 0.052(5) -0.014(4) 0.004(4) -0.010(5) C8 0.054(6) 0.118(8) 0.077(6) 0.014(6) -0.008(6) -0.006(6) C9 0.064(7) 0.135(9) 0.108(8) 0.004(7) 0.011(6) 0.033(7) C10 0.057(8) 0.058(7) 0.082(8) -0.012(7) 0.000(6) 0.003(6) C11 0.057(6) 0.062(7) 0.078(7) -0.028(5) 0.010(6) -0.004(5) C12 0.074(8) 0.080(10) 0.105(9) -0.030(8) 0.021(7) -0.002(7) C13 0.061(7) 0.078(8) 0.105(7) 0.012(7) 0.024(7) 0.016(7) C14 0.121(9) 0.106(9) 0.104(8) 0.031(8) 0.021(7) 0.013(8) C15 0.159(11) 0.146(12) 0.124(8) 0.000(10) 0.011(9) 0.033(10) C16 0.061(7) 0.084(8) 0.072(7) -0.018(6) -0.011(6) -0.001(6) C17 0.062(7) 0.087(7) 0.088(7) -0.004(6) -0.023(7) 0.006(6) C18 0.032(6) 0.084(7) 0.057(6) -0.025(6) 0.007(5) -0.004(5) Cl7 0.1484(18) 0.1079(15) 0.0607(10) -0.0106(9) 0.0201(11) -0.0171(13) Cl8 0.0983(14) 0.0878(14) 0.1335(17) 0.0048(11) 0.0170(12) -0.0063(11) Cl9 0.1402(18) 0.1130(15) 0.0784(12) 0.0238(10) -0.0300(12) -0.0133(13) C19 0.105(5) 0.051(3) 0.060(3) 0.007(3) 0.004(3) -0.014(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 O1 2.080(3) . y Mo1 Cl4 2.4679(11) . y Mo1 Cl3 2.4694(11) . y Mo1 Cl1 2.4706(11) . y Mo1 Cl2 2.4721(11) . y Mo1 Mo3 2.5986(6) . ? Mo1 Mo2 2.5988(5) . ? Mo1 Mo2 2.6005(6) 3_556 ? Mo1 Mo3 2.6008(6) 3_556 ? Mo2 Cl5 2.4103(11) . y Mo2 Cl3 2.4746(11) . ? Mo2 Cl4 2.4759(12) . ? Mo2 Cl1 2.4776(12) 3_556 ? Mo2 Cl2 2.4804(11) 3_556 ? Mo2 Mo1 2.6005(6) 3_556 ? Mo2 Mo3 2.6028(6) . ? Mo2 Mo3 2.6051(6) 3_556 ? Mo3 Cl6 2.4220(12) . y Mo3 Cl4 2.4712(11) . ? Mo3 Cl1 2.4712(11) . ? Mo3 Cl3 2.4713(11) 3_556 ? Mo3 Cl2 2.4790(11) 3_556 ? Mo3 Mo1 2.6008(6) 3_556 ? Mo3 Mo2 2.6051(6) 3_556 ? Cl1 Mo2 2.4776(12) 3_556 ? Cl2 Mo3 2.4790(11) 3_556 ? Cl2 Mo2 2.4804(11) 3_556 ? Cl3 Mo3 2.4713(11) 3_556 ? P1 O1 1.489(3) . y P1 C7 1.762(6) . ? P1 C10 1.787(6) . ? P1 C1 1.787(6) . ? P1 C13 1.796(7) . ? P1 C4 1.810(6) . ? P1 C16 1.820(6) . ? C1 C2 1.519(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.500(7) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.529(8) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.489(8) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.520(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.481(8) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.529(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.490(8) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.515(9) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.474(9) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.519(8) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.485(8) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? Cl7 C19 1.733(6) . ? Cl8 C19 1.736(6) . ? Cl9 C19 1.746(6) . ? C19 H19 1.0000 . ? 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 Cl4 90.67(10) . . y O1 Mo1 Cl3 91.89(10) . . y Cl4 Mo1 Cl3 90.15(4) . . y O1 Mo1 Cl1 92.10(10) . . y Cl4 Mo1 Cl1 89.74(4) . . y Cl3 Mo1 Cl1 176.01(4) . . y O1 Mo1 Cl2 93.05(10) . . y Cl4 Mo1 Cl2 176.28(4) . . y Cl3 Mo1 Cl2 89.79(4) . . y Cl1 Mo1 Cl2 90.07(4) . . y O1 Mo1 Mo3 134.09(10) . . ? Cl4 Mo1 Mo3 58.32(3) . . ? Cl3 Mo1 Mo3 118.47(3) . . ? Cl1 Mo1 Mo3 58.29(3) . . ? Cl2 Mo1 Mo3 118.61(3) . . ? O1 Mo1 Mo2 133.93(9) . . ? Cl4 Mo1 Mo2 58.44(3) . . ? Cl3 Mo1 Mo2 58.39(3) . . ? Cl1 Mo1 Mo2 118.38(3) . . ? Cl2 Mo1 Mo2 118.57(3) . . ? Mo3 Mo1 Mo2 60.103(15) . . ? O1 Mo1 Mo2 135.88(9) . 3_556 ? Cl4 Mo1 Mo2 118.44(3) . 3_556 ? Cl3 Mo1 Mo2 118.31(3) . 3_556 ? Cl1 Mo1 Mo2 58.43(3) . 3_556 ? Cl2 Mo1 Mo2 58.48(3) . 3_556 ? Mo3 Mo1 Mo2 60.140(13) . 3_556 ? Mo2 Mo1 Mo2 90.185(17) . 3_556 ? O1 Mo1 Mo3 135.70(10) . 3_556 ? Cl4 Mo1 Mo3 118.56(3) . 3_556 ? Cl3 Mo1 Mo3 58.27(3) . 3_556 ? Cl1 Mo1 Mo3 118.47(3) . 3_556 ? Cl2 Mo1 Mo3 58.44(3) . 3_556 ? Mo3 Mo1 Mo3 90.188(16) . 3_556 ? Mo2 Mo1 Mo3 60.134(15) . 3_556 ? Mo2 Mo1 Mo3 60.054(14) 3_556 3_556 ? Cl5 Mo2 Cl3 92.42(4) . . ? Cl5 Mo2 Cl4 91.19(4) . . ? Cl3 Mo2 Cl4 89.84(4) . . ? Cl5 Mo2 Cl1 93.40(4) . 3_556 ? Cl3 Mo2 Cl1 89.90(4) . 3_556 ? Cl4 Mo2 Cl1 175.41(4) . 3_556 ? Cl5 Mo2 Cl2 92.09(4) . 3_556 ? Cl3 Mo2 Cl2 175.49(4) . 3_556 ? Cl4 Mo2 Cl2 90.18(4) . 3_556 ? Cl1 Mo2 Cl2 89.72(4) 3_556 3_556 ? Cl5 Mo2 Mo1 134.39(4) . . ? Cl3 Mo2 Mo1 58.19(3) . . ? Cl4 Mo2 Mo1 58.14(3) . . ? Cl1 Mo2 Mo1 118.07(3) 3_556 . ? Cl2 Mo2 Mo1 118.24(3) 3_556 . ? Cl5 Mo2 Mo1 135.78(4) . 3_556 ? Cl3 Mo2 Mo1 118.03(3) . 3_556 ? Cl4 Mo2 Mo1 118.12(3) . 3_556 ? Cl1 Mo2 Mo1 58.16(3) 3_556 3_556 ? Cl2 Mo2 Mo1 58.17(3) 3_556 3_556 ? Mo1 Mo2 Mo1 89.815(17) . 3_556 ? Cl5 Mo2 Mo3 134.12(4) . . ? Cl3 Mo2 Mo3 118.12(3) . . ? Cl4 Mo2 Mo3 58.17(3) . . ? Cl1 Mo2 Mo3 118.13(3) 3_556 . ? Cl2 Mo2 Mo3 58.32(3) 3_556 . ? Mo1 Mo2 Mo3 59.945(16) . . ? Mo1 Mo2 Mo3 59.978(16) 3_556 . ? Cl5 Mo2 Mo3 135.87(4) . 3_556 ? Cl3 Mo2 Mo3 58.16(3) . 3_556 ? Cl4 Mo2 Mo3 118.09(3) . 3_556 ? Cl1 Mo2 Mo3 58.12(3) 3_556 3_556 ? Cl2 Mo2 Mo3 118.05(3) 3_556 3_556 ? Mo1 Mo2 Mo3 59.971(16) . 3_556 ? Mo1 Mo2 Mo3 59.894(16) 3_556 3_556 ? Mo3 Mo2 Mo3 90.003(18) . 3_556 ? Cl6 Mo3 Cl4 91.56(4) . . ? Cl6 Mo3 Cl1 92.90(4) . . ? Cl4 Mo3 Cl1 89.65(4) . . ? Cl6 Mo3 Cl3 92.77(4) . 3_556 ? Cl4 Mo3 Cl3 175.67(4) . 3_556 ? Cl1 Mo3 Cl3 90.13(4) . 3_556 ? Cl6 Mo3 Cl2 91.40(4) . 3_556 ? Cl4 Mo3 Cl2 90.32(4) . 3_556 ? Cl1 Mo3 Cl2 175.70(4) . 3_556 ? Cl3 Mo3 Cl2 89.58(4) 3_556 3_556 ? Cl6 Mo3 Mo1 135.20(4) . . ? Cl4 Mo3 Mo1 58.19(3) . . ? Cl1 Mo3 Mo1 58.26(3) . . ? Cl3 Mo3 Mo1 118.22(3) 3_556 . ? Cl2 Mo3 Mo1 118.30(3) 3_556 . ? Cl6 Mo3 Mo1 134.97(4) . 3_556 ? Cl4 Mo3 Mo1 118.29(3) . 3_556 ? Cl1 Mo3 Mo1 118.23(3) . 3_556 ? Cl3 Mo3 Mo1 58.20(3) 3_556 3_556 ? Cl2 Mo3 Mo1 58.18(3) 3_556 3_556 ? Mo1 Mo3 Mo1 89.812(16) . 3_556 ? Cl6 Mo3 Mo2 134.02(3) . . ? Cl4 Mo3 Mo2 58.35(3) . . ? Cl1 Mo3 Mo2 118.20(3) . . ? Cl3 Mo3 Mo2 118.16(3) 3_556 . ? Cl2 Mo3 Mo2 58.37(3) 3_556 . ? Mo1 Mo3 Mo2 59.951(13) . . ? Mo1 Mo3 Mo2 59.968(16) 3_556 . ? Cl6 Mo3 Mo2 135.98(3) . 3_556 ? Cl4 Mo3 Mo2 118.15(3) . 3_556 ? Cl1 Mo3 Mo2 58.36(3) . 3_556 ? Cl3 Mo3 Mo2 58.28(3) 3_556 3_556 ? Cl2 Mo3 Mo2 118.07(3) 3_556 3_556 ? Mo1 Mo3 Mo2 59.966(15) . 3_556 ? Mo1 Mo3 Mo2 59.894(15) 3_556 3_556 ? Mo2 Mo3 Mo2 89.997(18) . 3_556 ? Mo1 Cl1 Mo3 63.45(3) . . ? Mo1 Cl1 Mo2 63.41(3) . 3_556 ? Mo3 Cl1 Mo2 63.53(3) . 3_556 ? Mo1 Cl2 Mo3 63.38(3) . 3_556 ? Mo1 Cl2 Mo2 63.35(3) . 3_556 ? Mo3 Cl2 Mo2 63.31(3) 3_556 3_556 ? Mo1 Cl3 Mo3 63.52(3) . 3_556 ? Mo1 Cl3 Mo2 63.42(3) . . ? Mo3 Cl3 Mo2 63.57(3) 3_556 . ? Mo1 Cl4 Mo3 63.49(3) . . ? Mo1 Cl4 Mo2 63.43(3) . . ? Mo3 Cl4 Mo2 63.49(3) . . ? O1 P1 C7 110.4(3) . . ? O1 P1 C10 107.3(4) . . ? O1 P1 C1 113.5(4) . . ? C7 P1 C1 110.4(3) . . ? O1 P1 C13 117.2(4) . . ? C10 P1 C13 109.2(4) . . ? O1 P1 C4 106.9(4) . . ? C7 P1 C4 108.4(3) . . ? C1 P1 C4 107.0(3) . . ? O1 P1 C16 110.9(4) . . ? C10 P1 C16 106.4(4) . . ? C13 P1 C16 105.3(4) . . ? P1 O1 Mo1 171.1(2) . . y C2 C1 P1 116.9(5) . . ? C2 C1 H1A 108.1 . . ? P1 C1 H1A 108.1 . . ? C2 C1 H1B 108.1 . . ? P1 C1 H1B 108.1 . . ? H1A C1 H1B 107.3 . . ? C3 C2 C1 113.5(6) . . ? C3 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? C3 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 P1 115.2(5) . . ? C5 C4 H4A 108.5 . . ? P1 C4 H4A 108.5 . . ? C5 C4 H4B 108.5 . . ? P1 C4 H4B 108.5 . . ? H4A C4 H4B 107.5 . . ? C6 C5 C4 112.5(7) . . ? C6 C5 H5A 109.1 . . ? C4 C5 H5A 109.1 . . ? C6 C5 H5B 109.1 . . ? C4 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 P1 110.1(6) . . ? C8 C7 H7A 109.6 . . ? P1 C7 H7A 109.6 . . ? C8 C7 H7B 109.6 . . ? P1 C7 H7B 109.6 . . ? H7A C7 H7B 108.2 . . ? C9 C8 C7 114.5(7) . . ? C9 C8 H8A 108.6 . . ? C7 C8 H8A 108.6 . . ? C9 C8 H8B 108.6 . . ? C7 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 P1 112.5(6) . . ? C11 C10 H10A 109.1 . . ? P1 C10 H10A 109.1 . . ? C11 C10 H10B 109.1 . . ? P1 C10 H10B 109.1 . . ? H10A C10 H10B 107.8 . . ? C12 C11 C10 113.3(8) . . ? C12 C11 H11A 108.9 . . ? C10 C11 H11A 108.9 . . ? C12 C11 H11B 108.9 . . ? C10 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 P1 111.7(9) . . ? C14 C13 H13A 109.3 . . ? P1 C13 H13A 109.3 . . ? C14 C13 H13B 109.3 . . ? P1 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? C15 C14 C13 114.4(8) . . ? C15 C14 H14A 108.7 . . ? C13 C14 H14A 108.7 . . ? C15 C14 H14B 108.6 . . ? C13 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 P1 121.1(8) . . ? C17 C16 H16A 107.1 . . ? P1 C16 H16A 107.1 . . ? C17 C16 H16B 107.1 . . ? P1 C16 H16B 107.1 . . ? H16A C16 H16B 106.8 . . ? C18 C17 C16 112.6(7) . . ? C18 C17 H17A 109.1 . . ? C16 C17 H17A 109.1 . . ? C18 C17 H17B 109.1 . . ? C16 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Cl7 C19 Cl8 110.2(3) . . ? Cl7 C19 Cl9 111.2(3) . . ? Cl8 C19 Cl9 110.1(3) . . ? Cl7 C19 H19 108.4 . . ? Cl8 C19 H19 108.4 . . ? Cl9 C19 H19 108.4 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.582 _refine_diff_density_min -0.576 _refine_diff_density_rms 0.094 _publ_requested_category CM loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1.00 0.00 1.00 0.0300 -1.00 0.00 -1.00 0.0300 0.00 1.00 -1.00 0.0800 0.00 -1.00 1.00 0.0800 1.00 -1.00 0.00 0.1000 -1.00 1.00 0.00 0.1000