# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Guido Pampaloni' _publ_contact_author_email PAMPA@DCCI.UNIPI.IT _publ_section_title ; A Systematic Study on the Activation of Simple Polyethers by MoCl5 and WCl6 ; loop_ _publ_author_name 'Guido Pampaloni' 'Sara Dolci' 'Fabio Marchetti' 'Stefano Zacchini' # Attachment 'MoCl5-dioxolane1.cif' data_c2c _database_code_depnum_ccdc_archive 'CCDC 758020' #TrackingRef 'MoCl5-dioxolane1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C6 H10 Cl8 Mo2 O6' _chemical_formula_weight 653.62 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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.043(4) _cell_length_b 6.1669(10) _cell_length_c 14.915(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.412(2) _cell_angle_gamma 90.00 _cell_volume 1932.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6258 _cell_measurement_theta_min 2.3055 _cell_measurement_theta_max 28.451 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 2.421 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6562 _exptl_absorpt_correction_T_max 0.7766 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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 '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 6369 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1900 _reflns_number_gt 1871 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0101P)^2^+3.6331P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1900 _refine_ls_number_parameters 103 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0188 _refine_ls_R_factor_gt 0.0181 _refine_ls_wR_factor_ref 0.0417 _refine_ls_wR_factor_gt 0.0414 _refine_ls_goodness_of_fit_ref 1.176 _refine_ls_restrained_S_all 1.176 _refine_ls_shift/su_max 0.003 _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 0.452968(8) 1.09494(3) 1.092720(11) 0.01262(6) Uani 1 1 d . . . Cl1 Cl 0.51371(2) 0.76816(8) 1.05354(3) 0.01500(11) Uani 1 1 d . . . Cl2 Cl 0.40644(3) 0.88982(8) 1.19997(3) 0.02275(12) Uani 1 1 d . . . Cl3 Cl 0.37498(2) 1.35985(8) 1.09464(4) 0.02029(12) Uani 1 1 d . . . Cl4 Cl 0.29048(3) 0.33538(8) 0.86135(4) 0.02299(12) Uani 1 1 d . . . O1 O 0.51172(7) 1.2159(2) 1.15184(10) 0.0198(3) Uani 1 1 d . . . O2 O 0.38422(7) 0.9250(2) 0.99045(10) 0.0159(3) Uani 1 1 d . . . C1 C 0.32705(10) 0.8975(3) 0.99209(16) 0.0211(5) Uani 1 1 d D . . H1 H 0.3035(11) 0.927(4) 1.0416(12) 0.025 Uiso 1 1 d D . . O3 O 0.29161(7) 0.8133(2) 0.92565(10) 0.0207(3) Uani 1 1 d . . . C2 C 0.32296(10) 0.7595(3) 0.84419(13) 0.0189(4) Uani 1 1 d . . . H2A H 0.3569 0.8669 0.8347 0.023 Uiso 1 1 calc R . . H2B H 0.2917 0.7662 0.7920 0.023 Uiso 1 1 calc R . . C3 C 0.35133(10) 0.5372(4) 0.85077(15) 0.0200(4) Uani 1 1 d . . . H3A H 0.3821 0.5299 0.9036 0.024 Uiso 1 1 calc R . . H3B H 0.3747 0.5072 0.7964 0.024 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 0.01347(10) 0.01360(10) 0.01096(10) -0.00143(6) 0.00222(6) -0.00276(6) Cl1 0.0156(2) 0.0157(2) 0.0140(2) 0.00187(18) 0.00334(17) 0.00026(18) Cl2 0.0318(3) 0.0209(3) 0.0168(2) -0.0013(2) 0.0120(2) -0.0067(2) Cl3 0.0198(2) 0.0177(2) 0.0238(3) -0.0050(2) 0.0050(2) 0.00097(19) Cl4 0.0240(3) 0.0166(2) 0.0281(3) -0.0039(2) -0.0007(2) -0.0027(2) O1 0.0207(8) 0.0222(8) 0.0162(7) -0.0005(6) -0.0012(6) -0.0048(6) O2 0.0131(7) 0.0172(7) 0.0175(7) -0.0023(6) 0.0024(5) -0.0025(6) C1 0.0180(11) 0.0196(11) 0.0264(11) -0.0092(9) 0.0071(9) -0.0044(8) O3 0.0133(7) 0.0197(7) 0.0292(8) -0.0092(7) 0.0013(6) -0.0037(6) C2 0.0216(11) 0.0211(11) 0.0137(10) 0.0023(8) -0.0027(8) -0.0024(9) C3 0.0168(10) 0.0216(11) 0.0218(11) -0.0047(9) 0.0038(8) -0.0024(9) _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 1.6532(14) . ? Mo1 O2 2.2924(14) . ? Mo1 Cl2 2.3029(6) . ? Mo1 Cl3 2.3170(6) . ? Mo1 Cl1 2.4749(6) . ? Mo1 Cl1 2.4790(6) 5_677 ? Cl1 Mo1 2.4790(6) 5_677 ? Cl4 C3 1.799(2) . ? O2 C1 1.217(3) . ? C1 O3 1.311(3) . ? C1 H1 0.932(10) . ? O3 C2 1.455(3) . ? C2 C3 1.496(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? 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 169.59(6) . . ? O1 Mo1 Cl2 102.28(5) . . ? O2 Mo1 Cl2 86.19(4) . . ? O1 Mo1 Cl3 100.54(6) . . ? O2 Mo1 Cl3 84.91(4) . . ? Cl2 Mo1 Cl3 92.75(2) . . ? O1 Mo1 Cl1 96.50(6) . . ? O2 Mo1 Cl1 77.58(4) . . ? Cl2 Mo1 Cl1 87.92(2) . . ? Cl3 Mo1 Cl1 162.395(19) . . ? O1 Mo1 Cl1 94.24(5) . 5_677 ? O2 Mo1 Cl1 76.74(4) . 5_677 ? Cl2 Mo1 Cl1 162.266(19) . 5_677 ? Cl3 Mo1 Cl1 90.479(19) . 5_677 ? Cl1 Mo1 Cl1 83.826(18) . 5_677 ? Mo1 Cl1 Mo1 96.174(18) . 5_677 ? C1 O2 Mo1 129.49(14) . . ? O2 C1 O3 123.9(2) . . ? O2 C1 H1 124.3(16) . . ? O3 C1 H1 111.7(16) . . ? C1 O3 C2 117.11(16) . . ? O3 C2 C3 110.68(17) . . ? O3 C2 H2A 109.5 . . ? C3 C2 H2A 109.5 . . ? O3 C2 H2B 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C2 C3 Cl4 110.87(15) . . ? C2 C3 H3A 109.5 . . ? Cl4 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? Cl4 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? 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 O1 Mo1 Cl1 Mo1 -93.59(5) . . . 5_677 ? O2 Mo1 Cl1 Mo1 77.73(4) . . . 5_677 ? Cl2 Mo1 Cl1 Mo1 164.28(2) . . . 5_677 ? Cl3 Mo1 Cl1 Mo1 71.75(6) . . . 5_677 ? Cl1 Mo1 Cl1 Mo1 0.0 5_677 . . 5_677 ? O1 Mo1 O2 C1 -166.7(3) . . . . ? Cl2 Mo1 O2 C1 48.54(18) . . . . ? Cl3 Mo1 O2 C1 -44.57(18) . . . . ? Cl1 Mo1 O2 C1 137.24(19) . . . . ? Cl1 Mo1 O2 C1 -136.27(19) 5_677 . . . ? Mo1 O2 C1 O3 173.94(14) . . . . ? O2 C1 O3 C2 -2.8(3) . . . . ? C1 O3 C2 C3 86.3(2) . . . . ? O3 C2 C3 Cl4 62.64(19) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.303 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.086 # Attachment 'MoCl5-CH2_OET_21.cif' data_p21c _database_code_depnum_ccdc_archive 'CCDC 758021' #TrackingRef 'MoCl5-CH2_OET_21.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C5 H15 Cl5 Mo2 O5' _chemical_formula_weight 524.30 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' 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 P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7518(9) _cell_length_b 12.8342(9) _cell_length_c 10.3363(7) _cell_angle_alpha 90.00 _cell_angle_beta 109.0410(10) _cell_angle_gamma 90.00 _cell_volume 1599.07(19) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9979 _cell_measurement_theta_min 2.214 _cell_measurement_theta_max 28.4335 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.178 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1016 _exptl_absorpt_coefficient_mu 2.406 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6994 _exptl_absorpt_correction_T_max 0.7777 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _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 '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 15987 _diffrn_reflns_av_R_equivalents 0.0159 _diffrn_reflns_av_sigmaI/netI 0.0115 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 26.00 _reflns_number_total 3142 _reflns_number_gt 3016 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0160P)^2^+2.9919P] 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 3142 _refine_ls_number_parameters 154 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0199 _refine_ls_R_factor_gt 0.0188 _refine_ls_wR_factor_ref 0.0468 _refine_ls_wR_factor_gt 0.0460 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.004 _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 C1 C 0.5806(3) 0.8819(2) 0.5303(3) 0.0327(7) Uani 1 1 d U . . H1A H 0.5320 0.8487 0.5746 0.049 Uiso 1 1 calc R . . H1B H 0.6210 0.8282 0.4983 0.049 Uiso 1 1 calc R . . H1C H 0.5357 0.9234 0.4521 0.049 Uiso 1 1 calc R . . C2 C 0.9981(2) 0.9135(2) 0.7129(3) 0.0263(6) Uani 1 1 d U . . H2A H 1.0093 0.8410 0.6907 0.039 Uiso 1 1 calc R . . H2B H 1.0181 0.9212 0.8124 0.039 Uiso 1 1 calc R . . H2C H 1.0448 0.9593 0.6791 0.039 Uiso 1 1 calc R . . C3 C 0.7224(2) 1.26271(19) 0.7006(3) 0.0264(6) Uani 1 1 d U . . H3A H 0.6508 1.2988 0.6734 0.040 Uiso 1 1 calc R . . H3B H 0.7754 1.3031 0.6704 0.040 Uiso 1 1 calc R . . H3C H 0.7505 1.2554 0.8004 0.040 Uiso 1 1 calc R . . C4 C 0.5362(2) 1.1009(2) 0.8895(3) 0.0258(6) Uani 1 1 d U . . H4A H 0.5115 1.1698 0.8506 0.039 Uiso 1 1 calc R . . H4B H 0.5679 1.1064 0.9893 0.039 Uiso 1 1 calc R . . H4C H 0.4728 1.0531 0.8655 0.039 Uiso 1 1 calc R . . C5 C 0.8148(3) 0.7388(2) 0.9145(4) 0.0490(10) Uani 1 1 d U . . H5A H 0.8708 0.7030 0.8847 0.073 Uiso 1 1 calc R . . H5B H 0.7465 0.6973 0.8888 0.073 Uiso 1 1 calc R . . H5C H 0.8426 0.7476 1.0141 0.073 Uiso 1 1 calc R . . Cl1 Cl 0.87077(5) 1.06778(5) 0.87671(6) 0.01974(12) Uani 1 1 d U . . Cl2 Cl 0.71428(5) 1.03012(5) 0.38789(6) 0.02061(13) Uani 1 1 d U . . Cl3 Cl 0.92235(5) 1.15927(5) 0.59848(7) 0.02355(13) Uani 1 1 d U . . Cl4 Cl 0.75258(6) 0.94912(5) 1.07704(6) 0.02719(14) Uani 1 1 d U . . Cl5 Cl 0.55801(5) 0.84314(4) 0.82014(6) 0.01852(12) Uani 1 1 d U . . Mo1 Mo 0.783477(16) 1.044301(14) 0.62546(2) 0.01244(6) Uani 1 1 d U . . Mo2 Mo 0.710403(16) 0.955788(15) 0.83423(2) 0.01254(6) Uani 1 1 d U . . O1 O 0.65844(13) 0.94875(12) 0.62686(16) 0.0133(2) Uani 1 1 d U . . O2 O 0.88538(14) 0.94092(12) 0.65040(17) 0.0162(3) Uani 1 1 d U . . O3 O 0.70872(14) 1.16202(12) 0.63887(17) 0.0166(3) Uani 1 1 d U . . O4 O 0.61759(14) 1.06261(13) 0.83604(17) 0.0165(3) Uani 1 1 d U . . O5 O 0.79211(14) 0.83807(13) 0.85070(18) 0.0192(3) Uani 1 1 d U . . 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 C1 0.0394(16) 0.0421(17) 0.0184(10) -0.0117(11) 0.0117(11) -0.0276(12) C2 0.0175(10) 0.0306(14) 0.0301(14) -0.0011(11) 0.0067(10) 0.0073(9) C3 0.0255(13) 0.0125(9) 0.0410(16) -0.0067(10) 0.0107(12) 0.0017(9) C4 0.0281(14) 0.0258(14) 0.0310(14) 0.0029(11) 0.0201(11) 0.0102(10) C5 0.0434(19) 0.0298(14) 0.089(3) 0.0358(17) 0.0417(19) 0.0218(13) Cl1 0.0178(3) 0.0218(3) 0.0190(3) -0.0034(2) 0.0051(2) -0.0037(2) Cl2 0.0291(3) 0.0190(3) 0.0147(3) 0.0018(2) 0.0085(2) -0.0015(2) Cl3 0.0232(3) 0.0190(3) 0.0338(3) -0.0009(2) 0.0166(3) -0.0068(2) Cl4 0.0284(3) 0.0389(4) 0.0138(3) 0.0012(2) 0.0064(2) 0.0001(3) Cl5 0.0176(3) 0.0173(3) 0.0238(3) 0.0027(2) 0.0109(2) -0.0017(2) Mo1 0.01408(10) 0.01013(10) 0.01476(11) -0.00055(7) 0.00697(8) -0.00097(7) Mo2 0.01279(10) 0.01255(10) 0.01326(10) -0.00019(7) 0.00558(8) 0.00052(7) O1 0.0145(6) 0.0121(6) 0.0142(4) -0.0013(5) 0.0061(4) -0.0023(4) O2 0.0158(6) 0.0151(6) 0.0202(7) 0.0003(6) 0.0092(5) 0.0021(5) O3 0.0184(7) 0.0104(5) 0.0228(7) -0.0004(5) 0.0093(6) 0.0005(5) O4 0.0192(7) 0.0141(6) 0.0197(7) -0.0011(6) 0.0114(6) 0.0017(5) O5 0.0184(7) 0.0162(6) 0.0261(8) 0.0069(5) 0.0115(7) 0.0051(5) _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 C1 O1 1.439(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 O2 1.414(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 O3 1.426(3) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 O4 1.413(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 O5 1.421(3) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? Cl1 Mo2 2.4196(6) . ? Cl1 Mo1 2.4876(6) . ? Cl2 Mo1 2.3297(6) . ? Cl3 Mo1 2.3902(6) . ? Cl4 Mo2 2.3905(7) . ? Cl5 Mo2 2.3881(6) . ? Mo1 O3 1.8157(16) . ? Mo1 O2 1.8157(16) . ? Mo1 O1 2.0154(16) . ? Mo1 Mo2 2.8509(3) . ? Mo2 O5 1.8115(16) . ? Mo2 O4 1.8153(16) . ? Mo2 O1 2.0285(16) . ? 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 C1 H1A 109.5 . . ? O1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? O1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O2 C2 H2A 109.5 . . ? O2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? O2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O3 C3 H3A 109.5 . . ? O3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? O3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O4 C4 H4A 109.5 . . ? O4 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? O4 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O5 C5 H5A 109.5 . . ? O5 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? O5 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Mo2 Cl1 Mo1 71.020(17) . . ? O3 Mo1 O2 165.11(8) . . ? O3 Mo1 O1 93.98(7) . . ? O2 Mo1 O1 94.91(7) . . ? O3 Mo1 Cl2 96.76(6) . . ? O2 Mo1 Cl2 95.74(6) . . ? O1 Mo1 Cl2 86.08(5) . . ? O3 Mo1 Cl3 85.56(5) . . ? O2 Mo1 Cl3 86.82(5) . . ? O1 Mo1 Cl3 173.99(5) . . ? Cl2 Mo1 Cl3 88.02(2) . . ? O3 Mo1 Cl1 83.50(6) . . ? O2 Mo1 Cl1 83.37(6) . . ? O1 Mo1 Cl1 98.73(5) . . ? Cl2 Mo1 Cl1 175.16(2) . . ? Cl3 Mo1 Cl1 87.18(2) . . ? O3 Mo1 Mo2 87.96(5) . . ? O2 Mo1 Mo2 89.82(5) . . ? O1 Mo1 Mo2 45.36(5) . . ? Cl2 Mo1 Mo2 131.434(18) . . ? Cl3 Mo1 Mo2 140.521(18) . . ? Cl1 Mo1 Mo2 53.378(15) . . ? O5 Mo2 O4 170.37(7) . . ? O5 Mo2 O1 92.39(7) . . ? O4 Mo2 O1 93.17(7) . . ? O5 Mo2 Cl5 86.13(6) . . ? O4 Mo2 Cl5 86.42(5) . . ? O1 Mo2 Cl5 85.97(5) . . ? O5 Mo2 Cl4 86.90(6) . . ? O4 Mo2 Cl4 86.58(6) . . ? O1 Mo2 Cl4 172.66(5) . . ? Cl5 Mo2 Cl4 86.69(2) . . ? O5 Mo2 Cl1 92.99(6) . . ? O4 Mo2 Cl1 93.71(6) . . ? O1 Mo2 Cl1 100.58(5) . . ? Cl5 Mo2 Cl1 173.42(2) . . ? Cl4 Mo2 Cl1 86.75(2) . . ? O5 Mo2 Mo1 94.79(5) . . ? O4 Mo2 Mo1 94.71(5) . . ? O1 Mo2 Mo1 44.99(4) . . ? Cl5 Mo2 Mo1 130.958(17) . . ? Cl4 Mo2 Mo1 142.354(19) . . ? Cl1 Mo2 Mo1 55.602(15) . . ? C1 O1 Mo1 136.55(15) . . ? C1 O1 Mo2 132.32(15) . . ? Mo1 O1 Mo2 89.66(6) . . ? C2 O2 Mo1 145.09(16) . . ? C3 O3 Mo1 142.87(16) . . ? C4 O4 Mo2 146.20(16) . . ? C5 O5 Mo2 144.63(18) . . ? 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 Mo2 Cl1 Mo1 O3 92.30(5) . . . . ? Mo2 Cl1 Mo1 O2 -94.73(5) . . . . ? Mo2 Cl1 Mo1 O1 -0.76(5) . . . . ? Mo2 Cl1 Mo1 Cl2 -174.4(3) . . . . ? Mo2 Cl1 Mo1 Cl3 178.15(2) . . . . ? Mo1 Cl1 Mo2 O5 93.75(6) . . . . ? Mo1 Cl1 Mo2 O4 -93.17(5) . . . . ? Mo1 Cl1 Mo2 O1 0.76(5) . . . . ? Mo1 Cl1 Mo2 Cl5 175.90(18) . . . . ? Mo1 Cl1 Mo2 Cl4 -179.52(2) . . . . ? O3 Mo1 Mo2 O5 -173.77(8) . . . . ? O2 Mo1 Mo2 O5 -8.49(8) . . . . ? O1 Mo1 Mo2 O5 88.60(8) . . . . ? Cl2 Mo1 Mo2 O5 89.02(6) . . . . ? Cl3 Mo1 Mo2 O5 -93.26(6) . . . . ? Cl1 Mo1 Mo2 O5 -90.35(6) . . . . ? O3 Mo1 Mo2 O4 7.87(7) . . . . ? O2 Mo1 Mo2 O4 173.14(7) . . . . ? O1 Mo1 Mo2 O4 -89.77(8) . . . . ? Cl2 Mo1 Mo2 O4 -89.35(6) . . . . ? Cl3 Mo1 Mo2 O4 88.37(6) . . . . ? Cl1 Mo1 Mo2 O4 91.28(6) . . . . ? O3 Mo1 Mo2 O1 97.64(8) . . . . ? O2 Mo1 Mo2 O1 -97.09(8) . . . . ? Cl2 Mo1 Mo2 O1 0.42(6) . . . . ? Cl3 Mo1 Mo2 O1 178.14(7) . . . . ? Cl1 Mo1 Mo2 O1 -178.95(6) . . . . ? O3 Mo1 Mo2 Cl5 97.21(6) . . . . ? O2 Mo1 Mo2 Cl5 -97.52(6) . . . . ? O1 Mo1 Mo2 Cl5 -0.43(6) . . . . ? Cl2 Mo1 Mo2 Cl5 -0.01(3) . . . . ? Cl3 Mo1 Mo2 Cl5 177.71(3) . . . . ? Cl1 Mo1 Mo2 Cl5 -179.38(3) . . . . ? O3 Mo1 Mo2 Cl4 -82.64(6) . . . . ? O2 Mo1 Mo2 Cl4 82.64(6) . . . . ? O1 Mo1 Mo2 Cl4 179.73(7) . . . . ? Cl2 Mo1 Mo2 Cl4 -179.85(3) . . . . ? Cl3 Mo1 Mo2 Cl4 -2.13(4) . . . . ? Cl1 Mo1 Mo2 Cl4 0.78(3) . . . . ? O3 Mo1 Mo2 Cl1 -83.41(6) . . . . ? O2 Mo1 Mo2 Cl1 81.86(6) . . . . ? O1 Mo1 Mo2 Cl1 178.95(6) . . . . ? Cl2 Mo1 Mo2 Cl1 179.37(3) . . . . ? Cl3 Mo1 Mo2 Cl1 -2.91(3) . . . . ? O3 Mo1 O1 C1 110.3(3) . . . . ? O2 Mo1 O1 C1 -81.7(3) . . . . ? Cl2 Mo1 O1 C1 13.8(2) . . . . ? Cl3 Mo1 O1 C1 24.8(6) . . . . ? Cl1 Mo1 O1 C1 -165.7(2) . . . . ? Mo2 Mo1 O1 C1 -166.6(3) . . . . ? O3 Mo1 O1 Mo2 -83.17(7) . . . . ? O2 Mo1 O1 Mo2 84.88(7) . . . . ? Cl2 Mo1 O1 Mo2 -179.68(5) . . . . ? Cl3 Mo1 O1 Mo2 -168.6(4) . . . . ? Cl1 Mo1 O1 Mo2 0.85(5) . . . . ? O5 Mo2 O1 C1 73.1(2) . . . . ? O4 Mo2 O1 C1 -99.0(2) . . . . ? Cl5 Mo2 O1 C1 -12.8(2) . . . . ? Cl4 Mo2 O1 C1 -11.2(5) . . . . ? Cl1 Mo2 O1 C1 166.6(2) . . . . ? Mo1 Mo2 O1 C1 167.5(3) . . . . ? O5 Mo2 O1 Mo1 -94.38(7) . . . . ? O4 Mo2 O1 Mo1 93.49(7) . . . . ? Cl5 Mo2 O1 Mo1 179.67(5) . . . . ? Cl4 Mo2 O1 Mo1 -178.7(3) . . . . ? Cl1 Mo2 O1 Mo1 -0.88(5) . . . . ? O3 Mo1 O2 C2 -17.9(5) . . . . ? O1 Mo1 O2 C2 -144.3(3) . . . . ? Cl2 Mo1 O2 C2 129.1(3) . . . . ? Cl3 Mo1 O2 C2 41.4(3) . . . . ? Cl1 Mo1 O2 C2 -46.1(3) . . . . ? Mo2 Mo1 O2 C2 -99.2(3) . . . . ? O2 Mo1 O3 C3 15.4(5) . . . . ? O1 Mo1 O3 C3 142.0(3) . . . . ? Cl2 Mo1 O3 C3 -131.5(3) . . . . ? Cl3 Mo1 O3 C3 -44.0(3) . . . . ? Cl1 Mo1 O3 C3 43.6(3) . . . . ? Mo2 Mo1 O3 C3 97.0(3) . . . . ? O5 Mo2 O4 C4 4.4(7) . . . . ? O1 Mo2 O4 C4 129.6(3) . . . . ? Cl5 Mo2 O4 C4 43.8(3) . . . . ? Cl4 Mo2 O4 C4 -43.1(3) . . . . ? Cl1 Mo2 O4 C4 -129.6(3) . . . . ? Mo1 Mo2 O4 C4 174.7(3) . . . . ? O4 Mo2 O5 C5 -3.7(7) . . . . ? O1 Mo2 O5 C5 -128.9(4) . . . . ? Cl5 Mo2 O5 C5 -43.1(4) . . . . ? Cl4 Mo2 O5 C5 43.8(4) . . . . ? Cl1 Mo2 O5 C5 130.3(4) . . . . ? Mo1 Mo2 O5 C5 -173.9(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.651 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.083