Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Drew, Michael G. B.' 'Felix, Vitor' 'Romao, C. C.' 'Royo, Beatriz' _publ_contact_author_name 'Prof.Vitor Felix' _publ_contact_author_address ; Departamento de Quimica, Universidade de Aveiro 3810 193 Aveiro Portugal ; _publ_contact_letter ; ; _publ_contact_author_phone '[351]234 370 729' _publ_contact_author_fax '[351]234 370 084' _publ_contact_author_email 'vfelix@dq.ua.pt or felix@itqb.unl.pt' _publ_section_title ; Bis-Indenyl Molybdenum(IV) Halide complexes: synthesis and X-ray studies ; #-------------------------- data section of block --------------------------- #======BEGIN data_compound_1_[Ind2Mo(CO)Br][BF4] _database_code_CSD 167778 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[Ind2Mo(CO)Br][BF4]' _chemical_formula_sum 'C19 H14 B Br F4 Mo O' _chemical_formula_weight 520.95 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.928(11) _cell_length_b 9.285(14) _cell_length_c 12.402(17) _cell_angle_alpha 96.67(1) _cell_angle_beta 97.05(1) _cell_angle_gamma 112.66(1) _cell_volume 926(1) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.867 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 508 _exptl_absorpt_coefficient_mu 2.908 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3186 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 26.06 _reflns_number_total 3186 _reflns_number_gt 2324 _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 w==1/[\s^2^(Fo^2^)+(0.1592P)^2^+1.0659P] 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 SHELXL _refine_ls_extinction_coef 0.003(3) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3186 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0910 _refine_ls_R_factor_gt 0.0655 _refine_ls_wR_factor_ref 0.2216 _refine_ls_wR_factor_gt 0.1893 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.78713(8) 0.68509(7) 0.73763(5) 0.0449(3) Uani 1 d . . . Br1 Br 0.67053(12) 0.81099(11) 0.58647(7) 0.0631(4) Uani 1 d . . . C100 C 0.5465(12) 0.5590(11) 0.7282(7) 0.061(2) Uani 1 d . . . O100 O 0.4079(8) 0.4846(10) 0.7231(7) 0.086(2) Uani 1 d . . . C11 C 0.7638(12) 0.7249(11) 0.9184(7) 0.062(2) Uani 1 d . . . H11 H 0.6935 0.6439 0.9490 0.075 Uiso 1 calc R . . C12 C 0.7211(10) 0.8338(10) 0.8654(6) 0.0528(18) Uani 1 d . . . H12 H 0.6149 0.8297 0.8484 0.063 Uiso 1 calc R . . C13 C 0.8664(9) 0.9511(9) 0.8419(6) 0.0465(16) Uani 1 d . . . C14 C 0.8958(12) 1.0926(10) 0.7998(7) 0.060(2) Uani 1 d . . . H14 H 0.8111 1.1245 0.7798 0.072 Uiso 1 calc R . . C15 C 1.0551(13) 1.1807(12) 0.7899(8) 0.066(2) Uani 1 d . . . H15 H 1.0782 1.2752 0.7634 0.080 Uiso 1 calc R . . C16 C 1.1828(13) 1.1350(11) 0.8177(7) 0.065(2) Uani 1 d . . . H16 H 1.2874 1.1992 0.8070 0.078 Uiso 1 calc R . . C17 C 1.1643(11) 1.0033(11) 0.8591(7) 0.060(2) Uani 1 d . . . H17 H 1.2531 0.9765 0.8782 0.072 Uiso 1 calc R . . C18 C 0.9982(10) 0.9045(10) 0.8726(6) 0.0512(18) Uani 1 d . . . C19 C 0.9326(10) 0.7605(10) 0.9169(6) 0.0515(18) Uani 1 d . . . H19 H 0.9905 0.7019 0.9403 0.062 Uiso 1 calc R . . C21 C 0.7709(13) 0.4334(10) 0.7014(8) 0.065(2) Uani 1 d . . . H21 H 0.6953 0.3524 0.7291 0.078 Uiso 1 calc R . . C22 C 0.7395(12) 0.4849(10) 0.5984(7) 0.060(2) Uani 1 d . . . H22 H 0.6384 0.4499 0.5510 0.071 Uiso 1 calc R . . C23 C 0.8938(11) 0.6002(10) 0.5837(6) 0.0558(19) Uani 1 d . . . C24 C 0.9390(13) 0.6873(12) 0.4953(7) 0.066(2) Uani 1 d . . . H24 H 0.8598 0.6725 0.4341 0.079 Uiso 1 calc R . . C25 C 1.0941(14) 0.7886(14) 0.5020(9) 0.080(3) Uani 1 d . . . H25 H 1.1240 0.8456 0.4455 0.096 Uiso 1 calc R . . C26 C 1.2181(14) 0.8104(15) 0.5986(10) 0.088(4) Uani 1 d . . . H26 H 1.3272 0.8782 0.6001 0.105 Uiso 1 calc R . . C27 C 1.1817(12) 0.7370(13) 0.6854(9) 0.071(3) Uani 1 d . . . H27 H 1.2612 0.7579 0.7478 0.085 Uiso 1 calc R . . C28 C 1.0153(11) 0.6256(11) 0.6772(7) 0.057(2) Uani 1 d . . . C29 C 0.9351(12) 0.5267(11) 0.7522(7) 0.062(2) Uani 1 d . . . H29 H 0.9839 0.5251 0.8225 0.075 Uiso 1 calc R . . B1 B 0.6591(14) 0.2995(14) 0.9769(11) 0.066(3) Uani 1 d . . . F11 F 0.6381(16) 0.227(2) 1.0568(12) 0.215(7) Uani 1 d . . . F12 F 0.5573(11) 0.3643(12) 0.9601(14) 0.193(7) Uani 1 d . . . F13 F 0.8179(8) 0.3928(10) 0.9730(8) 0.120(3) Uani 1 d . . . F14 F 0.602(2) 0.181(2) 0.8867(15) 0.260(10) Uani 1 d . . . 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 0.0450(4) 0.0443(5) 0.0469(4) 0.0079(3) 0.0126(3) 0.0185(3) Br1 0.0655(6) 0.0615(6) 0.0608(6) 0.0138(4) 0.0015(4) 0.0263(5) C100 0.062(5) 0.064(5) 0.057(5) 0.013(4) 0.011(4) 0.026(5) O100 0.048(4) 0.092(6) 0.104(6) 0.016(4) 0.017(4) 0.013(4) C11 0.080(6) 0.066(6) 0.046(4) 0.015(4) 0.027(4) 0.028(5) C12 0.046(4) 0.062(5) 0.050(4) 0.003(3) 0.016(3) 0.022(4) C13 0.045(4) 0.042(4) 0.052(4) 0.007(3) 0.017(3) 0.014(3) C14 0.064(5) 0.056(5) 0.064(5) 0.004(4) 0.014(4) 0.029(4) C15 0.076(6) 0.058(5) 0.067(5) 0.004(4) 0.016(5) 0.030(5) C16 0.073(6) 0.054(5) 0.062(5) 0.013(4) 0.019(4) 0.016(5) C17 0.055(5) 0.069(6) 0.053(5) 0.000(4) 0.014(4) 0.025(4) C18 0.053(4) 0.061(5) 0.044(4) 0.000(3) 0.016(3) 0.028(4) C19 0.064(5) 0.058(5) 0.042(4) 0.009(3) 0.011(3) 0.033(4) C21 0.085(7) 0.045(5) 0.073(6) 0.012(4) 0.036(5) 0.027(5) C22 0.061(5) 0.049(5) 0.065(5) -0.003(4) 0.020(4) 0.020(4) C23 0.061(5) 0.065(5) 0.044(4) 0.000(3) 0.013(3) 0.031(4) C24 0.079(6) 0.073(6) 0.052(5) 0.012(4) 0.026(4) 0.031(5) C25 0.084(7) 0.081(7) 0.074(6) 0.016(5) 0.037(6) 0.025(6) C26 0.068(6) 0.096(9) 0.092(8) -0.014(6) 0.038(6) 0.027(6) C27 0.053(5) 0.090(7) 0.068(6) -0.013(5) 0.009(4) 0.034(5) C28 0.061(5) 0.071(5) 0.051(4) 0.000(4) 0.015(4) 0.041(5) C29 0.078(6) 0.069(6) 0.062(5) 0.018(4) 0.019(4) 0.049(5) B1 0.057(6) 0.056(6) 0.098(8) 0.040(6) 0.038(6) 0.024(5) F11 0.138(9) 0.304(18) 0.218(13) 0.187(14) 0.050(9) 0.062(11) F12 0.072(5) 0.113(8) 0.40(2) 0.082(10) 0.047(8) 0.039(6) F13 0.053(3) 0.117(6) 0.199(8) 0.087(6) 0.037(4) 0.022(4) F14 0.212(15) 0.235(16) 0.28(2) -0.047(15) 0.142(14) 0.032(14) _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 C100 1.992(10) . ? Mo1 C22 2.254(8) . ? Mo1 C12 2.261(8) . ? Mo1 C21 2.272(8) . ? Mo1 C11 2.278(8) . ? Mo1 C19 2.313(8) . ? Mo1 C29 2.332(8) . ? Mo1 C23 2.418(8) . ? Mo1 C13 2.442(7) . ? Mo1 C18 2.445(8) . ? Mo1 C28 2.483(7) . ? Mo1 Br1 2.6329(10) . ? C100 O100 1.151(11) . ? C11 C12 1.411(12) . ? C11 C19 1.416(12) . ? C12 C13 1.425(11) . ? C13 C14 1.412(11) . ? C13 C18 1.428(11) . ? C14 C15 1.370(13) . ? C15 C16 1.381(14) . ? C16 C17 1.341(13) . ? C17 C18 1.456(12) . ? C18 C19 1.441(11) . ? C21 C29 1.401(14) . ? C21 C22 1.448(13) . ? C22 C23 1.431(13) . ? C23 C28 1.417(12) . ? C23 C24 1.442(12) . ? C24 C25 1.326(14) . ? C25 C26 1.466(17) . ? C26 C27 1.347(16) . ? C27 C28 1.429(13) . ? C28 C29 1.441(12) . ? B1 F11 1.253(14) . ? B1 F12 1.279(13) . ? B1 F13 1.358(12) . ? B1 F14 1.36(2) . ? 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 C100 Mo1 C22 79.2(4) . . ? C100 Mo1 C12 77.4(3) . . ? C22 Mo1 C12 156.4(3) . . ? C100 Mo1 C21 78.7(4) . . ? C22 Mo1 C21 37.3(3) . . ? C12 Mo1 C21 137.9(3) . . ? C100 Mo1 C11 79.0(4) . . ? C22 Mo1 C11 139.9(3) . . ? C12 Mo1 C11 36.2(3) . . ? C21 Mo1 C11 105.1(3) . . ? C100 Mo1 C19 112.8(3) . . ? C22 Mo1 C19 134.2(3) . . ? C12 Mo1 C19 60.0(3) . . ? C21 Mo1 C19 99.5(3) . . ? C11 Mo1 C19 35.9(3) . . ? C100 Mo1 C29 111.3(4) . . ? C22 Mo1 C29 60.4(3) . . ? C12 Mo1 C29 132.5(3) . . ? C21 Mo1 C29 35.4(4) . . ? C11 Mo1 C29 97.6(3) . . ? C19 Mo1 C29 74.5(3) . . ? C100 Mo1 C23 113.0(3) . . ? C22 Mo1 C23 35.5(3) . . ? C12 Mo1 C23 163.1(3) . . ? C21 Mo1 C23 58.9(3) . . ? C11 Mo1 C23 155.0(3) . . ? C19 Mo1 C23 122.7(3) . . ? C29 Mo1 C23 58.0(3) . . ? C100 Mo1 C13 109.7(3) . . ? C22 Mo1 C13 161.6(3) . . ? C12 Mo1 C13 35.0(3) . . ? C21 Mo1 C13 157.9(3) . . ? C11 Mo1 C13 58.6(3) . . ? C19 Mo1 C13 58.5(3) . . ? C29 Mo1 C13 126.4(3) . . ? C23 Mo1 C13 129.5(3) . . ? C100 Mo1 C18 133.8(3) . . ? C22 Mo1 C18 145.4(3) . . ? C12 Mo1 C18 58.0(3) . . ? C21 Mo1 C18 126.2(3) . . ? C11 Mo1 C18 58.2(3) . . ? C19 Mo1 C18 35.1(3) . . ? C29 Mo1 C18 92.4(3) . . ? C23 Mo1 C18 113.2(3) . . ? C13 Mo1 C18 34.0(3) . . ? C100 Mo1 C28 134.4(3) . . ? C22 Mo1 C28 58.3(3) . . ? C12 Mo1 C28 144.8(3) . . ? C21 Mo1 C28 57.8(3) . . ? C11 Mo1 C28 122.6(3) . . ? C19 Mo1 C28 89.1(3) . . ? C29 Mo1 C28 34.6(3) . . ? C23 Mo1 C28 33.6(3) . . ? C13 Mo1 C28 115.8(3) . . ? C18 Mo1 C28 87.2(3) . . ? C100 Mo1 Br1 80.8(3) . . ? C22 Mo1 Br1 85.5(2) . . ? C12 Mo1 Br1 87.8(2) . . ? C21 Mo1 Br1 121.8(3) . . ? C11 Mo1 Br1 123.4(2) . . ? C19 Mo1 Br1 138.7(2) . . ? C29 Mo1 Br1 139.0(2) . . ? C23 Mo1 Br1 81.1(2) . . ? C13 Mo1 Br1 80.24(18) . . ? C18 Mo1 Br1 107.0(2) . . ? C28 Mo1 Br1 109.2(2) . . ? O100 C100 Mo1 179.2(8) . . ? C12 C11 C19 108.0(7) . . ? C12 C11 Mo1 71.2(4) . . ? C19 C11 Mo1 73.4(4) . . ? C11 C12 C13 109.2(7) . . ? C11 C12 Mo1 72.5(5) . . ? C13 C12 Mo1 79.4(4) . . ? C14 C13 C18 120.8(7) . . ? C14 C13 C12 132.5(8) . . ? C18 C13 C12 106.7(7) . . ? C14 C13 Mo1 127.6(5) . . ? C18 C13 Mo1 73.1(4) . . ? C12 C13 Mo1 65.5(4) . . ? C15 C14 C13 116.9(8) . . ? C14 C15 C16 122.7(9) . . ? C17 C16 C15 123.7(9) . . ? C16 C17 C18 116.5(9) . . ? C13 C18 C19 108.2(7) . . ? C13 C18 C17 119.4(8) . . ? C19 C18 C17 132.3(8) . . ? C13 C18 Mo1 72.9(5) . . ? C19 C18 Mo1 67.4(4) . . ? C17 C18 Mo1 127.1(5) . . ? C11 C19 C18 107.4(7) . . ? C11 C19 Mo1 70.7(5) . . ? C18 C19 Mo1 77.4(4) . . ? C29 C21 C22 108.2(8) . . ? C29 C21 Mo1 74.6(5) . . ? C22 C21 Mo1 70.7(5) . . ? C23 C22 C21 106.8(8) . . ? C23 C22 Mo1 78.5(5) . . ? C21 C22 Mo1 72.0(5) . . ? C28 C23 C22 108.8(8) . . ? C28 C23 C24 119.6(9) . . ? C22 C23 C24 131.7(9) . . ? C28 C23 Mo1 75.7(4) . . ? C22 C23 Mo1 66.0(4) . . ? C24 C23 Mo1 124.3(6) . . ? C25 C24 C23 119.6(10) . . ? C24 C25 C26 119.8(10) . . ? C27 C26 C25 123.1(11) . . ? C26 C27 C28 117.0(10) . . ? C23 C28 C27 120.8(9) . . ? C23 C28 C29 107.4(8) . . ? C27 C28 C29 131.8(9) . . ? C23 C28 Mo1 70.7(4) . . ? C27 C28 Mo1 126.1(6) . . ? C29 C28 Mo1 66.9(4) . . ? C21 C29 C28 108.5(8) . . ? C21 C29 Mo1 70.0(5) . . ? C28 C29 Mo1 78.4(4) . . ? F11 B1 F12 112.3(13) . . ? F11 B1 F13 115.8(12) . . ? F12 B1 F13 114.8(9) . . ? F11 B1 F14 104.0(15) . . ? F12 B1 F14 100.3(14) . . ? F13 B1 F14 107.5(11) . . ? _diffrn_measured_fraction_theta_max 0.869 _diffrn_reflns_theta_full 26.06 _diffrn_measured_fraction_theta_full 0.869 _refine_diff_density_max 1.586 _refine_diff_density_min -0.952 _refine_diff_density_rms 0.166 #======END data_compound_3_Ind2MoBr2 _database_code_CSD 167779 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety Ind2MoBr2 _chemical_formula_sum 'C18 H14 Br2 Mo1' _chemical_formula_weight 486.05 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Br' 'Br' -0.2901 2.4595 '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/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 15.134(17) _cell_length_b 14.522(19) _cell_length_c 29.774(33) _cell_angle_alpha 90.00 _cell_angle_beta 104.27(1) _cell_angle_gamma 90.00 _cell_volume 6342(1) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.036 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3744 _exptl_absorpt_coefficient_mu 5.857 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20536 _diffrn_reflns_av_R_equivalents 0.0589 _diffrn_reflns_av_sigmaI/netI 0.0875 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 26.13 _reflns_number_total 11030 _reflns_number_gt 6709 _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 w==1/[\s^2^(Fo^2^)+(0.0841P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00002(3) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11030 _refine_ls_number_parameters 758 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1382 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1746 _refine_ls_wR_factor_gt 0.1437 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.28390(6) 0.88393(6) -0.00255(3) 0.0319(2) Uani 1 d . . . Br11 Br 0.30852(8) 1.01356(8) 0.06127(4) 0.0473(3) Uani 1 d . . . Br21 Br 0.33027(8) 1.01451(8) -0.05271(4) 0.0461(3) Uani 1 d . . . C191 C 0.3360(9) 0.7394(8) 0.0168(4) 0.054(4) Uani 1 d . . . H191 H 0.2921 0.6956 0.0186 0.065 Uiso 1 calc R . . C181 C 0.3717(7) 0.7563(7) -0.0224(4) 0.036(3) Uani 1 d . . . C171 C 0.3564(9) 0.7109(8) -0.0660(4) 0.054(3) Uani 1 d . . . H171 H 0.3123 0.6653 -0.0748 0.065 Uiso 1 calc R . . C161 C 0.4099(9) 0.7380(9) -0.0941(4) 0.060(4) Uani 1 d . . . H161 H 0.4032 0.7092 -0.1226 0.072 Uiso 1 calc R . . C151 C 0.4753(8) 0.8085(8) -0.0814(4) 0.046(3) Uani 1 d . . . H151 H 0.5121 0.8225 -0.1012 0.055 Uiso 1 calc R . . C141 C 0.4865(7) 0.8558(8) -0.0421(4) 0.040(3) Uani 1 d . . . H141 H 0.5268 0.9051 -0.0354 0.049 Uiso 1 calc R . . C131 C 0.4334(7) 0.8271(8) -0.0103(4) 0.038(3) Uani 1 d . . . C121 C 0.4345(7) 0.8618(8) 0.0351(3) 0.037(3) Uani 1 d . . . H121 H 0.4653 0.9131 0.0498 0.045 Uiso 1 calc R . . C111 C 0.3786(8) 0.8007(8) 0.0523(4) 0.050(3) Uani 1 d . . . H111 H 0.3710 0.8007 0.0823 0.060 Uiso 1 calc R . . C211 C 0.1632(7) 0.8651(9) -0.0639(4) 0.051(3) Uani 1 d . . . H211 H 0.1735 0.8655 -0.0934 0.061 Uiso 1 calc R . . C221 C 0.1655(8) 0.7882(8) -0.0353(4) 0.044(3) Uani 1 d . . . H221 H 0.1796 0.7283 -0.0421 0.052 Uiso 1 calc R . . C231 C 0.1423(7) 0.8176(8) 0.0061(4) 0.035(3) Uani 1 d . . . C241 C 0.1308(8) 0.7677(10) 0.0452(4) 0.055(3) Uani 1 d . . . H241 H 0.1448 0.7054 0.0489 0.066 Uiso 1 calc R . . C251 C 0.0983(8) 0.8159(10) 0.0768(4) 0.056(4) Uani 1 d . . . H251 H 0.0885 0.7846 0.1024 0.068 Uiso 1 calc R . . C261 C 0.0790(8) 0.9088(11) 0.0731(4) 0.058(4) Uani 1 d . . . H261 H 0.0571 0.9378 0.0960 0.070 Uiso 1 calc R . . C271 C 0.0914(8) 0.9580(9) 0.0370(5) 0.052(3) Uani 1 d . . . H271 H 0.0787 1.0208 0.0349 0.062 Uiso 1 calc R . . C281 C 0.1237(7) 0.9132(7) 0.0022(4) 0.035(3) Uani 1 d . . . C291 C 0.1421(7) 0.9420(9) -0.0394(4) 0.048(3) Uani 1 d . . . H291 H 0.1406 1.0028 -0.0495 0.058 Uiso 1 calc R . . Mo2 Mo 0.71423(6) 0.87379(6) 0.48883(3) 0.0314(2) Uani 1 d . . . Br12 Br 0.70097(9) 1.01123(8) 0.43064(4) 0.0495(3) Uani 1 d . . . Br22 Br 0.68543(9) 1.00352(9) 0.54516(4) 0.0528(4) Uani 1 d . . . C112 C 0.8324(8) 0.8340(9) 0.5478(4) 0.050(3) Uani 1 d . . . H112 H 0.8230 0.8293 0.5774 0.060 Uiso 1 calc R . . C122 C 0.8608(7) 0.9132(9) 0.5284(4) 0.046(3) Uani 1 d . . . H122 H 0.8664 0.9719 0.5413 0.056 Uiso 1 calc R . . C132 C 0.8796(7) 0.8880(8) 0.4859(4) 0.041(3) Uani 1 d . . . C142 C 0.9184(7) 0.9381(9) 0.4538(4) 0.045(3) Uani 1 d . . . H142 H 0.9350 0.9996 0.4589 0.054 Uiso 1 calc R . . C152 C 0.9300(8) 0.8926(10) 0.4158(4) 0.056(3) Uani 1 d . . . H152 H 0.9613 0.9212 0.3964 0.068 Uiso 1 calc R . . C162 C 0.8953(8) 0.8027(8) 0.4052(4) 0.046(3) Uani 1 d . . . H162 H 0.9000 0.7759 0.3775 0.056 Uiso 1 calc R . . C172 C 0.8564(8) 0.7550(8) 0.4331(4) 0.043(3) Uani 1 d . . . H172 H 0.8348 0.6957 0.4253 0.052 Uiso 1 calc R . . C182 C 0.8484(8) 0.7962(7) 0.4752(4) 0.036(3) Uani 1 d . . . C192 C 0.8205(8) 0.7626(8) 0.5146(4) 0.044(3) Uani 1 d . . . H192 H 0.7983 0.7039 0.5179 0.052 Uiso 1 calc R . . C212 C 0.6069(8) 0.8096(8) 0.4304(4) 0.049(3) Uani 1 d . . . H212 H 0.6127 0.8151 0.4001 0.059 Uiso 1 calc R . . C222 C 0.5611(8) 0.8721(8) 0.4526(4) 0.047(3) Uani 1 d . . . H222 H 0.5358 0.9283 0.4411 0.056 Uiso 1 calc R . . C232 C 0.5609(7) 0.8323(7) 0.4969(4) 0.035(3) Uani 1 d . . . C242 C 0.5179(8) 0.8595(9) 0.5323(4) 0.055(3) Uani 1 d . . . H242 H 0.4827 0.9126 0.5296 0.066 Uiso 1 calc R . . C252 C 0.5310(8) 0.8040(10) 0.5703(4) 0.058(4) Uani 1 d . . . H252 H 0.5028 0.8200 0.5937 0.070 Uiso 1 calc R . . C262 C 0.5844(9) 0.7245(11) 0.5761(5) 0.065(4) Uani 1 d . . . H262 H 0.5889 0.6887 0.6025 0.078 Uiso 1 calc R . . C272 C 0.6289(9) 0.6986(9) 0.5451(5) 0.061(4) Uani 1 d . . . H272 H 0.6690 0.6491 0.5507 0.073 Uiso 1 calc R . . C282 C 0.6133(8) 0.7498(8) 0.5021(4) 0.043(3) Uani 1 d . . . C292 C 0.6421(8) 0.7383(8) 0.4605(4) 0.046(3) Uani 1 d . . . H292 H 0.6787 0.6907 0.4544 0.055 Uiso 1 calc R . . Mo3 Mo 0.36251(6) 0.72311(6) 0.22171(3) 0.0332(2) Uani 1 d . . . Br13 Br 0.49223(9) 0.70038(9) 0.17722(4) 0.0545(4) Uani 1 d . . . Br23 Br 0.49929(8) 0.69474(8) 0.29500(4) 0.0451(3) Uani 1 d . . . C113 C 0.2973(9) 0.6135(9) 0.1710(4) 0.056(4) Uani 1 d . . . H113 H 0.3054 0.6167 0.1410 0.067 Uiso 1 calc R . . C123 C 0.2244(7) 0.6520(8) 0.1863(4) 0.047(3) Uani 1 d . . . H123 H 0.1773 0.6873 0.1686 0.056 Uiso 1 calc R . . C133 C 0.2352(8) 0.6276(8) 0.2337(4) 0.040(3) Uani 1 d . . . C143 C 0.1819(9) 0.6448(9) 0.2652(5) 0.055(3) Uani 1 d . . . H143 H 0.1308 0.6826 0.2569 0.066 Uiso 1 calc R . . C153 C 0.2053(10) 0.6064(10) 0.3073(5) 0.064(4) Uani 1 d . . . H153 H 0.1703 0.6181 0.3283 0.077 Uiso 1 calc R . . C163 C 0.2815(11) 0.5490(10) 0.3201(5) 0.064(4) Uani 1 d . . . H163 H 0.2927 0.5199 0.3488 0.077 Uiso 1 calc R . . C173 C 0.3407(9) 0.5332(9) 0.2926(4) 0.058(4) Uani 1 d . . . H173 H 0.3937 0.4987 0.3026 0.069 Uiso 1 calc R . . C183 C 0.3150(8) 0.5737(7) 0.2476(4) 0.045(3) Uani 1 d . . . C193 C 0.3566(9) 0.5686(8) 0.2096(4) 0.048(3) Uani 1 d . . . H193 H 0.4123 0.5410 0.2099 0.057 Uiso 1 calc R . . C213 C 0.3251(11) 0.8509(9) 0.1782(5) 0.063(4) Uani 1 d . . . H213 H 0.3184 0.8465 0.1464 0.076 Uiso 1 calc R . . C223 C 0.2559(8) 0.8376(8) 0.2020(4) 0.051(3) Uani 1 d . . . H223 H 0.1961 0.8192 0.1891 0.061 Uiso 1 calc R . . C233 C 0.2964(8) 0.8581(8) 0.2502(4) 0.045(3) Uani 1 d . . . C243 C 0.2565(11) 0.8614(9) 0.2882(5) 0.065(4) Uani 1 d . . . H243 H 0.1971 0.8415 0.2859 0.078 Uiso 1 calc R . . C253 C 0.3090(18) 0.8950(12) 0.3281(6) 0.104(8) Uani 1 d . . . H253 H 0.2832 0.9009 0.3533 0.125 Uiso 1 calc R . . C263 C 0.398(2) 0.9209(13) 0.3339(6) 0.123(11) Uani 1 d . . . H263 H 0.4304 0.9425 0.3626 0.148 Uiso 1 calc R . . C273 C 0.4383(11) 0.9156(9) 0.2989(6) 0.084(6) Uani 1 d . . . H273 H 0.4993 0.9320 0.3033 0.101 Uiso 1 calc R . . C283 C 0.3878(8) 0.8849(7) 0.2554(4) 0.049(3) Uani 1 d . . . C293 C 0.4061(10) 0.8723(9) 0.2116(5) 0.062(4) Uani 1 d . . . H293 H 0.4634 0.8773 0.2056 0.074 Uiso 1 calc R . . Mo4 Mo 0.62944(6) 1.28913(6) 0.27709(3) 0.0331(2) Uani 1 d . . . Br14 Br 0.49178(8) 1.30082(8) 0.20291(4) 0.0452(3) Uani 1 d . . . Br24 Br 0.49940(9) 1.31575(9) 0.32020(4) 0.0550(4) Uani 1 d . . . C214 C 0.6881(9) 1.4122(8) 0.3214(4) 0.052(3) Uani 1 d . . . H214 H 0.6783 1.4172 0.3509 0.063 Uiso 1 calc R . . C224 C 0.7631(8) 1.3720(8) 0.3107(4) 0.045(3) Uani 1 d . . . H224 H 0.8103 1.3419 0.3314 0.054 Uiso 1 calc R . . C234 C 0.7555(7) 1.3849(8) 0.2618(4) 0.039(3) Uani 1 d . . . C244 C 0.8150(8) 1.3613(8) 0.2329(4) 0.049(3) Uani 1 d . . . H244 H 0.8682 1.3279 0.2441 0.058 Uiso 1 calc R . . C254 C 0.7898(9) 1.3899(9) 0.1888(4) 0.055(4) Uani 1 d . . . H254 H 0.8279 1.3769 0.1694 0.066 Uiso 1 calc R . . C264 C 0.7087(9) 1.4387(9) 0.1704(4) 0.051(3) Uani 1 d . . . H264 H 0.6959 1.4584 0.1398 0.061 Uiso 1 calc R . . C274 C 0.6502(8) 1.4572(8) 0.1957(4) 0.044(3) Uani 1 d . . . H274 H 0.5950 1.4863 0.1827 0.052 Uiso 1 calc R . . C284 C 0.6741(8) 1.4311(7) 0.2433(3) 0.037(3) Uani 1 d . . . C294 C 0.6285(9) 1.4448(7) 0.2797(4) 0.043(3) Uani 1 d . . . H294 H 0.5708 1.4701 0.2767 0.052 Uiso 1 calc R . . C114 C 0.6756(9) 1.1755(8) 0.3264(5) 0.052(3) Uani 1 d . . . H114 H 0.6835 1.1902 0.3575 0.063 Uiso 1 calc R . . C134 C 0.7016(8) 1.1529(7) 0.2549(4) 0.042(3) Uani 1 d . . . C144 C 0.7381(9) 1.1417(8) 0.2155(5) 0.056(4) Uani 1 d . . . H144 H 0.7966 1.1618 0.2157 0.067 Uiso 1 calc R . . C124 C 0.7416(8) 1.1834(9) 0.3017(5) 0.055(3) Uani 1 d . . . H124 H 0.8009 1.2045 0.3132 0.066 Uiso 1 calc R . . C154 C 0.6842(13) 1.1005(9) 0.1775(5) 0.070(5) Uani 1 d . . . H154 H 0.7053 1.0953 0.1508 0.084 Uiso 1 calc R . . C164 C 0.5989(13) 1.0661(10) 0.1772(5) 0.078(5) Uani 1 d . . . H164 H 0.5684 1.0314 0.1519 0.094 Uiso 1 calc R . . C174 C 0.5581(9) 1.0805(8) 0.2120(5) 0.059(4) Uani 1 d . . . H174 H 0.4976 1.0643 0.2093 0.071 Uiso 1 calc R . . C184 C 0.6122(8) 1.1219(7) 0.2531(4) 0.043(3) Uani 1 d . . . C194 C 0.5934(10) 1.1414(8) 0.2967(4) 0.059(4) Uani 1 d . . . H194 H 0.5379 1.1334 0.3044 0.070 Uiso 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 0.0310(5) 0.0295(5) 0.0363(5) -0.0019(4) 0.0104(4) -0.0010(4) Br11 0.0435(7) 0.0465(8) 0.0547(7) -0.0175(6) 0.0176(6) -0.0022(6) Br21 0.0488(8) 0.0384(7) 0.0523(7) 0.0089(5) 0.0150(6) -0.0018(6) C191 0.086(10) 0.022(7) 0.070(9) 0.009(6) 0.046(8) 0.015(6) C181 0.040(7) 0.027(6) 0.043(6) 0.002(5) 0.014(5) 0.002(5) C171 0.058(9) 0.037(7) 0.070(9) -0.012(6) 0.021(7) -0.008(6) C161 0.057(9) 0.068(10) 0.060(9) -0.023(7) 0.024(7) -0.001(7) C151 0.047(8) 0.046(8) 0.052(8) -0.002(6) 0.025(6) 0.012(6) C141 0.025(6) 0.045(7) 0.051(7) 0.002(5) 0.008(5) 0.003(5) C131 0.032(7) 0.041(7) 0.042(7) 0.008(5) 0.014(5) 0.022(5) C121 0.030(6) 0.046(7) 0.032(6) -0.003(5) 0.003(5) 0.015(5) C111 0.061(9) 0.050(8) 0.048(8) 0.018(6) 0.029(6) 0.021(7) C211 0.032(7) 0.076(10) 0.045(7) -0.017(7) 0.011(5) -0.007(7) C221 0.040(7) 0.038(7) 0.056(7) -0.016(6) 0.020(6) -0.014(6) C231 0.020(6) 0.047(7) 0.041(6) -0.009(5) 0.013(5) -0.014(5) C241 0.046(8) 0.065(9) 0.059(8) 0.000(7) 0.023(6) -0.012(7) C251 0.035(8) 0.077(11) 0.057(8) -0.003(7) 0.011(6) -0.019(7) C261 0.027(7) 0.099(12) 0.051(8) -0.040(8) 0.015(6) -0.020(7) C271 0.036(7) 0.042(8) 0.083(10) -0.021(7) 0.025(7) 0.004(6) C281 0.020(6) 0.036(7) 0.048(7) 0.001(5) 0.003(5) 0.007(5) C291 0.019(6) 0.062(9) 0.060(8) 0.029(6) 0.002(5) 0.005(6) Mo2 0.0347(6) 0.0264(5) 0.0339(5) -0.0016(4) 0.0099(4) 0.0004(4) Br12 0.0528(8) 0.0399(7) 0.0582(8) 0.0125(6) 0.0187(6) -0.0002(6) Br22 0.0586(9) 0.0454(8) 0.0562(8) -0.0186(6) 0.0175(6) 0.0031(6) C112 0.040(7) 0.073(9) 0.037(7) 0.008(6) 0.010(5) 0.038(7) C122 0.032(7) 0.058(8) 0.050(7) -0.007(6) 0.012(5) 0.000(6) C132 0.030(7) 0.053(8) 0.040(7) 0.000(5) 0.010(5) 0.002(6) C142 0.020(6) 0.053(8) 0.058(8) 0.001(6) 0.002(5) -0.009(5) C152 0.035(7) 0.076(10) 0.056(8) 0.008(7) 0.009(6) -0.004(7) C162 0.044(8) 0.050(8) 0.046(7) 0.008(6) 0.013(6) 0.013(6) C172 0.054(8) 0.035(7) 0.046(7) 0.001(5) 0.023(6) 0.005(6) C182 0.046(7) 0.025(6) 0.040(6) 0.001(4) 0.016(5) 0.010(5) C192 0.050(8) 0.033(7) 0.049(7) 0.014(5) 0.013(6) 0.020(6) C212 0.058(9) 0.052(8) 0.037(7) -0.011(6) 0.009(6) -0.028(6) C222 0.052(8) 0.046(8) 0.038(7) 0.004(5) 0.004(5) -0.005(6) C232 0.030(6) 0.035(7) 0.042(6) -0.003(5) 0.012(5) -0.007(5) C242 0.047(8) 0.049(8) 0.077(10) 0.000(7) 0.032(7) 0.002(6) C252 0.032(7) 0.096(12) 0.051(8) -0.012(7) 0.019(6) -0.012(7) C262 0.040(8) 0.104(13) 0.055(9) 0.014(8) 0.022(6) 0.000(8) C272 0.047(8) 0.062(9) 0.073(9) 0.033(7) 0.014(7) 0.008(7) C282 0.045(8) 0.032(7) 0.060(8) 0.000(5) 0.025(6) -0.008(5) C292 0.057(8) 0.037(7) 0.048(7) -0.009(6) 0.022(6) -0.016(6) Mo3 0.0314(6) 0.0344(6) 0.0354(5) -0.0013(4) 0.0117(4) 0.0021(4) Br13 0.0512(8) 0.0651(9) 0.0568(8) -0.0039(6) 0.0316(6) 0.0037(7) Br23 0.0373(7) 0.0473(8) 0.0494(7) 0.0015(5) 0.0081(5) -0.0023(5) C113 0.056(9) 0.059(9) 0.056(8) -0.008(6) 0.020(7) -0.037(7) C123 0.023(6) 0.060(8) 0.050(7) 0.010(6) -0.007(5) -0.005(6) C133 0.041(7) 0.037(7) 0.043(7) 0.012(5) 0.012(5) -0.009(6) C143 0.050(8) 0.056(9) 0.064(9) -0.015(7) 0.025(7) -0.014(7) C153 0.075(11) 0.072(10) 0.058(9) -0.020(7) 0.042(8) -0.033(9) C163 0.078(11) 0.059(10) 0.056(9) -0.014(7) 0.018(8) -0.045(9) C173 0.049(9) 0.044(8) 0.071(9) 0.010(7) -0.002(7) -0.006(6) C183 0.035(7) 0.027(6) 0.070(8) -0.004(6) 0.011(6) 0.000(5) C193 0.054(8) 0.043(8) 0.047(7) -0.013(5) 0.013(6) -0.002(6) C213 0.108(13) 0.040(8) 0.048(8) 0.008(6) 0.031(8) 0.033(8) C223 0.035(7) 0.050(8) 0.060(8) -0.012(6) -0.003(6) 0.018(6) C233 0.052(8) 0.030(7) 0.058(8) 0.005(5) 0.021(6) 0.008(6) C243 0.086(11) 0.040(8) 0.088(11) 0.001(7) 0.057(9) 0.011(8) C253 0.21(3) 0.051(12) 0.056(12) 0.012(9) 0.050(15) 0.053(15) C263 0.23(3) 0.051(12) 0.055(11) -0.026(9) -0.026(16) 0.065(16) C273 0.063(10) 0.040(9) 0.114(13) -0.034(9) -0.047(10) 0.017(7) C283 0.047(8) 0.014(6) 0.081(9) -0.002(6) 0.004(7) 0.002(5) C293 0.072(10) 0.041(8) 0.086(10) 0.004(7) 0.044(9) -0.011(7) Mo4 0.0336(6) 0.0322(5) 0.0354(5) 0.0062(4) 0.0120(4) 0.0005(4) Br14 0.0376(7) 0.0491(8) 0.0479(7) 0.0070(5) 0.0087(5) -0.0006(6) Br24 0.0543(9) 0.0633(9) 0.0576(8) 0.0071(6) 0.0333(6) 0.0046(7) C214 0.066(9) 0.052(8) 0.042(7) -0.006(6) 0.019(6) -0.017(7) C224 0.041(7) 0.045(7) 0.045(7) 0.003(5) 0.003(5) -0.015(6) C234 0.036(7) 0.041(7) 0.038(6) 0.016(5) 0.003(5) -0.004(6) C244 0.028(7) 0.049(8) 0.075(9) 0.015(6) 0.023(6) -0.001(6) C254 0.072(10) 0.051(8) 0.054(8) -0.009(6) 0.035(7) -0.023(7) C264 0.063(9) 0.064(9) 0.027(6) 0.012(6) 0.014(6) -0.014(7) C274 0.040(7) 0.035(7) 0.052(7) 0.010(5) 0.004(6) -0.011(5) C284 0.044(7) 0.034(7) 0.036(6) 0.003(5) 0.016(5) -0.010(5) C294 0.057(8) 0.030(6) 0.050(7) 0.006(5) 0.028(6) 0.001(6) C114 0.054(9) 0.033(7) 0.068(8) 0.013(6) 0.010(7) 0.010(6) C134 0.044(7) 0.028(6) 0.059(8) 0.003(5) 0.020(6) 0.010(5) C144 0.060(9) 0.036(7) 0.082(10) 0.021(7) 0.039(8) 0.012(7) C124 0.033(7) 0.054(9) 0.076(9) 0.009(7) 0.007(7) 0.005(6) C154 0.132(16) 0.040(9) 0.046(9) 0.018(6) 0.036(9) 0.018(9) C164 0.124(16) 0.039(9) 0.064(10) -0.005(7) 0.007(10) 0.025(10) C174 0.050(9) 0.023(7) 0.094(11) -0.002(7) -0.002(8) 0.008(6) C184 0.055(8) 0.024(6) 0.050(7) 0.013(5) 0.016(6) 0.012(6) C194 0.079(10) 0.040(8) 0.069(9) 0.024(6) 0.041(8) -0.002(7) _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 C111 2.242(11) . ? Mo1 C211 2.260(11) . ? Mo1 C191 2.266(11) . ? Mo1 C221 2.288(11) . ? Mo1 C121 2.301(10) . ? Mo1 C291 2.315(10) . ? Mo1 C231 2.421(9) . ? Mo1 C181 2.438(10) . ? Mo1 C131 2.472(10) . ? Mo1 C281 2.499(10) . ? Mo1 Br21 2.6143(14) . ? Mo1 Br11 2.6353(14) . ? C191 C111 1.411(17) . ? C191 C181 1.423(14) . ? C181 C131 1.375(15) . ? C181 C171 1.423(15) . ? C171 C161 1.357(16) . ? C161 C151 1.408(16) . ? C151 C141 1.330(14) . ? C141 C131 1.446(14) . ? C131 C121 1.438(14) . ? C121 C111 1.407(15) . ? C211 C221 1.399(16) . ? C211 C291 1.413(16) . ? C221 C231 1.430(14) . ? C231 C281 1.414(14) . ? C231 C241 1.415(15) . ? C241 C251 1.361(17) . ? C251 C261 1.378(18) . ? C261 C271 1.342(17) . ? C271 C281 1.409(14) . ? C281 C291 1.400(14) . ? Mo2 C112 2.251(11) . ? Mo2 C212 2.268(11) . ? Mo2 C192 2.275(10) . ? Mo2 C222 2.303(12) . ? Mo2 C292 2.307(11) . ? Mo2 C122 2.313(11) . ? Mo2 C182 2.442(10) . ? Mo2 C282 2.456(11) . ? Mo2 C232 2.466(10) . ? Mo2 C132 2.534(11) . ? Mo2 Br12 2.6181(14) . ? Mo2 Br22 2.6291(14) . ? C112 C122 1.400(17) . ? C112 C192 1.414(16) . ? C122 C132 1.411(14) . ? C132 C182 1.424(15) . ? C132 C142 1.436(15) . ? C142 C152 1.358(16) . ? C152 C162 1.415(17) . ? C162 C172 1.327(15) . ? C172 C182 1.420(14) . ? C182 C192 1.428(14) . ? C212 C292 1.387(16) . ? C212 C222 1.404(16) . ? C222 C232 1.439(14) . ? C232 C242 1.424(14) . ? C232 C282 1.424(15) . ? C242 C252 1.364(17) . ? C252 C262 1.395(18) . ? C262 C272 1.326(17) . ? C272 C282 1.447(15) . ? C282 C292 1.422(14) . ? Mo3 C113 2.248(12) . ? Mo3 C213 2.254(12) . ? Mo3 C193 2.271(11) . ? Mo3 C223 2.290(11) . ? Mo3 C293 2.305(12) . ? Mo3 C123 2.337(11) . ? Mo3 C233 2.445(11) . ? Mo3 C183 2.469(11) . ? Mo3 C133 2.469(10) . ? Mo3 C283 2.546(11) . ? Mo3 Br23 2.6438(15) . ? Mo3 Br13 2.6458(14) . ? C113 C123 1.410(17) . ? C113 C193 1.431(17) . ? C123 C133 1.422(14) . ? C133 C143 1.403(15) . ? C133 C183 1.413(15) . ? C143 C153 1.337(18) . ? C153 C163 1.40(2) . ? C163 C173 1.375(18) . ? C173 C183 1.425(16) . ? C183 C193 1.426(16) . ? C213 C293 1.409(19) . ? C213 C223 1.415(17) . ? C223 C233 1.446(16) . ? C233 C283 1.409(16) . ? C233 C243 1.410(16) . ? C243 C253 1.35(2) . ? C253 C263 1.36(3) . ? C263 C273 1.34(3) . ? C273 C283 1.404(17) . ? C283 C293 1.410(17) . ? Mo4 C114 2.204(11) . ? Mo4 C294 2.262(11) . ? Mo4 C214 2.269(12) . ? Mo4 C124 2.273(12) . ? Mo4 C194 2.324(11) . ? Mo4 C224 2.355(11) . ? Mo4 C134 2.429(10) . ? Mo4 C284 2.461(10) . ? Mo4 C234 2.492(10) . ? Mo4 C184 2.527(11) . ? Mo4 Br24 2.6297(14) . ? Mo4 Br14 2.6415(15) . ? C214 C224 1.381(16) . ? C214 C294 1.423(16) . ? C224 C234 1.446(14) . ? C234 C284 1.391(15) . ? C234 C244 1.431(15) . ? C244 C254 1.339(16) . ? C254 C264 1.405(17) . ? C264 C274 1.323(16) . ? C274 C284 1.426(14) . ? C284 C294 1.436(14) . ? C114 C124 1.383(16) . ? C114 C194 1.425(18) . ? C134 C184 1.415(16) . ? C134 C144 1.424(15) . ? C134 C124 1.446(16) . ? C144 C154 1.360(19) . ? C154 C164 1.38(2) . ? C164 C174 1.346(19) . ? C174 C184 1.428(17) . ? C184 C194 1.423(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 C111 Mo1 C211 140.2(5) . . ? C111 Mo1 C191 36.5(4) . . ? C211 Mo1 C191 104.7(5) . . ? C111 Mo1 C221 106.0(5) . . ? C211 Mo1 C221 35.8(4) . . ? C191 Mo1 C221 74.5(5) . . ? C111 Mo1 C121 36.0(4) . . ? C211 Mo1 C121 152.0(4) . . ? C191 Mo1 C121 60.4(5) . . ? C221 Mo1 C121 134.4(4) . . ? C111 Mo1 C291 153.3(4) . . ? C211 Mo1 C291 36.0(4) . . ? C191 Mo1 C291 133.0(5) . . ? C221 Mo1 C291 58.8(4) . . ? C121 Mo1 C291 166.6(4) . . ? C111 Mo1 C231 97.6(4) . . ? C211 Mo1 C231 58.5(4) . . ? C191 Mo1 C231 82.3(4) . . ? C221 Mo1 C231 35.2(3) . . ? C121 Mo1 C231 133.6(4) . . ? C291 Mo1 C231 56.9(4) . . ? C111 Mo1 C181 58.5(4) . . ? C211 Mo1 C181 95.3(4) . . ? C191 Mo1 C181 35.0(4) . . ? C221 Mo1 C181 81.4(4) . . ? C121 Mo1 C181 58.5(4) . . ? C291 Mo1 C181 131.2(4) . . ? C231 Mo1 C181 105.9(4) . . ? C111 Mo1 C131 56.8(4) . . ? C211 Mo1 C131 117.4(4) . . ? C191 Mo1 C131 56.3(4) . . ? C221 Mo1 C131 113.3(4) . . ? C121 Mo1 C131 34.8(3) . . ? C291 Mo1 C131 147.1(4) . . ? C231 Mo1 C131 137.0(4) . . ? C181 Mo1 C131 32.5(3) . . ? C111 Mo1 C281 120.3(4) . . ? C211 Mo1 C281 57.6(4) . . ? C191 Mo1 C281 115.1(4) . . ? C221 Mo1 C281 57.2(4) . . ? C121 Mo1 C281 148.7(3) . . ? C291 Mo1 C281 33.5(3) . . ? C231 Mo1 C281 33.4(3) . . ? C181 Mo1 C281 137.5(4) . . ? C131 Mo1 C281 170.0(4) . . ? C111 Mo1 Br21 126.4(3) . . ? C211 Mo1 Br21 84.5(3) . . ? C191 Mo1 Br21 133.7(3) . . ? C221 Mo1 Br21 119.3(3) . . ? C121 Mo1 Br21 90.4(3) . . ? C291 Mo1 Br21 79.2(3) . . ? C231 Mo1 Br21 136.0(3) . . ? C181 Mo1 Br21 100.0(2) . . ? C131 Mo1 Br21 78.9(3) . . ? C281 Mo1 Br21 108.1(2) . . ? C111 Mo1 Br11 84.8(3) . . ? C211 Mo1 Br11 127.7(3) . . ? C191 Mo1 Br11 120.0(3) . . ? C221 Mo1 Br11 134.3(3) . . ? C121 Mo1 Br11 78.6(3) . . ? C291 Mo1 Br11 91.8(3) . . ? C231 Mo1 Br11 100.3(2) . . ? C181 Mo1 Br11 136.9(3) . . ? C131 Mo1 Br11 109.6(3) . . ? C281 Mo1 Br11 78.7(2) . . ? Br21 Mo1 Br11 83.32(5) . . ? C111 C191 C181 108.0(11) . . ? C111 C191 Mo1 70.9(6) . . ? C181 C191 Mo1 79.1(6) . . ? C131 C181 C191 106.5(10) . . ? C131 C181 C171 122.2(10) . . ? C191 C181 C171 131.2(11) . . ? C131 C181 Mo1 75.1(6) . . ? C191 C181 Mo1 65.9(6) . . ? C171 C181 Mo1 126.7(8) . . ? C161 C171 C181 116.0(11) . . ? C171 C161 C151 122.1(11) . . ? C141 C151 C161 122.7(11) . . ? C151 C141 C131 117.1(11) . . ? C181 C131 C121 111.0(9) . . ? C181 C131 C141 119.7(10) . . ? C121 C131 C141 129.3(11) . . ? C181 C131 Mo1 72.4(6) . . ? C121 C131 Mo1 66.1(5) . . ? C141 C131 Mo1 129.4(7) . . ? C111 C121 C131 104.6(10) . . ? C111 C121 Mo1 69.7(6) . . ? C131 C121 Mo1 79.1(6) . . ? C121 C111 C191 109.3(10) . . ? C121 C111 Mo1 74.3(6) . . ? C191 C111 Mo1 72.7(7) . . ? C221 C211 C291 107.0(10) . . ? C221 C211 Mo1 73.2(7) . . ? C291 C211 Mo1 74.2(6) . . ? C211 C221 C231 108.2(10) . . ? C211 C221 Mo1 71.0(6) . . ? C231 C221 Mo1 77.5(6) . . ? C281 C231 C241 120.6(10) . . ? C281 C231 C221 107.9(9) . . ? C241 C231 C221 131.4(11) . . ? C281 C231 Mo1 76.3(6) . . ? C241 C231 Mo1 125.6(8) . . ? C221 C231 Mo1 67.3(6) . . ? C251 C241 C231 116.3(13) . . ? C241 C251 C261 123.5(13) . . ? C271 C261 C251 121.2(11) . . ? C261 C271 C281 118.9(12) . . ? C291 C281 C271 133.8(11) . . ? C291 C281 C231 106.8(9) . . ? C271 C281 C231 119.4(10) . . ? C291 C281 Mo1 66.0(6) . . ? C271 C281 Mo1 129.7(8) . . ? C231 C281 Mo1 70.3(6) . . ? C281 C291 C211 109.9(11) . . ? C281 C291 Mo1 80.4(6) . . ? C211 C291 Mo1 69.9(6) . . ? C112 Mo2 C212 140.7(5) . . ? C112 Mo2 C192 36.4(4) . . ? C212 Mo2 C192 106.3(5) . . ? C112 Mo2 C222 151.3(4) . . ? C212 Mo2 C222 35.8(4) . . ? C192 Mo2 C222 134.2(4) . . ? C112 Mo2 C292 106.2(5) . . ? C212 Mo2 C292 35.3(4) . . ? C192 Mo2 C292 75.5(4) . . ? C222 Mo2 C292 59.3(4) . . ? C112 Mo2 C122 35.7(4) . . ? C212 Mo2 C122 155.3(4) . . ? C192 Mo2 C122 59.6(4) . . ? C222 Mo2 C122 165.8(4) . . ? C292 Mo2 C122 134.8(5) . . ? C112 Mo2 C182 58.5(4) . . ? C212 Mo2 C182 98.6(4) . . ? C192 Mo2 C182 35.0(3) . . ? C222 Mo2 C182 134.4(4) . . ? C292 Mo2 C182 83.3(4) . . ? C122 Mo2 C182 57.7(4) . . ? C112 Mo2 C282 95.3(5) . . ? C212 Mo2 C282 57.7(4) . . ? C192 Mo2 C282 80.9(4) . . ? C222 Mo2 C282 58.2(4) . . ? C292 Mo2 C282 34.6(4) . . ? C122 Mo2 C282 131.0(4) . . ? C182 Mo2 C282 105.3(4) . . ? C112 Mo2 C232 116.6(4) . . ? C212 Mo2 C232 57.4(4) . . ? C192 Mo2 C232 113.4(4) . . ? C222 Mo2 C232 34.9(3) . . ? C292 Mo2 C232 57.0(4) . . ? C122 Mo2 C232 144.9(4) . . ? C182 Mo2 C232 138.1(4) . . ? C282 Mo2 C232 33.6(4) . . ? C112 Mo2 C132 56.4(4) . . ? C212 Mo2 C132 122.3(4) . . ? C192 Mo2 C132 56.5(4) . . ? C222 Mo2 C132 150.9(4) . . ? C292 Mo2 C132 116.0(4) . . ? C122 Mo2 C132 33.5(3) . . ? C182 Mo2 C132 33.2(3) . . ? C282 Mo2 C132 136.4(4) . . ? C232 Mo2 C132 169.9(4) . . ? C112 Mo2 Br12 128.9(4) . . ? C212 Mo2 Br12 83.2(3) . . ? C192 Mo2 Br12 134.2(3) . . ? C222 Mo2 Br12 78.1(3) . . ? C292 Mo2 Br12 117.1(3) . . ? C122 Mo2 Br12 93.2(3) . . ? C182 Mo2 Br12 100.0(2) . . ? C282 Mo2 Br12 135.8(3) . . ? C232 Mo2 Br12 109.3(3) . . ? C132 Mo2 Br12 80.2(3) . . ? C112 Mo2 Br22 84.9(3) . . ? C212 Mo2 Br22 125.7(3) . . ? C192 Mo2 Br22 120.5(3) . . ? C222 Mo2 Br22 90.0(3) . . ? C292 Mo2 Br22 135.0(3) . . ? C122 Mo2 Br22 77.7(3) . . ? C182 Mo2 Br22 135.4(3) . . ? C282 Mo2 Br22 102.4(3) . . ? C232 Mo2 Br22 78.7(2) . . ? C132 Mo2 Br22 106.5(3) . . ? Br12 Mo2 Br22 83.00(5) . . ? C122 C112 C192 108.3(10) . . ? C122 C112 Mo2 74.6(7) . . ? C192 C112 Mo2 72.7(6) . . ? C112 C122 C132 107.9(11) . . ? C112 C122 Mo2 69.7(7) . . ? C132 C122 Mo2 81.9(7) . . ? C122 C132 C182 108.3(10) . . ? C122 C132 C142 132.1(11) . . ? C182 C132 C142 119.5(10) . . ? C122 C132 Mo2 64.7(6) . . ? C182 C132 Mo2 69.9(6) . . ? C142 C132 Mo2 129.3(7) . . ? C152 C142 C132 117.8(11) . . ? C142 C152 C162 121.2(11) . . ? C172 C162 C152 122.6(11) . . ? C162 C172 C182 118.8(11) . . ? C172 C182 C132 119.7(10) . . ? C172 C182 C192 133.5(10) . . ? C132 C182 C192 106.6(9) . . ? C172 C182 Mo2 126.6(8) . . ? C132 C182 Mo2 76.9(6) . . ? C192 C182 Mo2 66.1(6) . . ? C112 C192 C182 108.1(10) . . ? C112 C192 Mo2 70.9(6) . . ? C182 C192 Mo2 78.9(6) . . ? C292 C212 C222 109.5(11) . . ? C292 C212 Mo2 73.9(7) . . ? C222 C212 Mo2 73.5(6) . . ? C212 C222 C232 106.6(11) . . ? C212 C222 Mo2 70.8(7) . . ? C232 C222 Mo2 78.8(6) . . ? C242 C232 C282 119.7(10) . . ? C242 C232 C222 132.1(11) . . ? C282 C232 C222 108.1(9) . . ? C242 C232 Mo2 128.1(8) . . ? C282 C232 Mo2 72.8(6) . . ? C222 C232 Mo2 66.3(6) . . ? C252 C242 C232 116.9(12) . . ? C242 C252 C262 123.5(11) . . ? C272 C262 C252 121.8(12) . . ? C262 C272 C282 118.0(12) . . ? C292 C282 C232 106.6(10) . . ? C292 C282 C272 133.7(12) . . ? C232 C282 C272 119.6(10) . . ? C292 C282 Mo2 67.0(6) . . ? C232 C282 Mo2 73.6(6) . . ? C272 C282 Mo2 123.1(9) . . ? C212 C292 C282 108.9(11) . . ? C212 C292 Mo2 70.8(6) . . ? C282 C292 Mo2 78.5(6) . . ? C113 Mo3 C213 101.0(5) . . ? C113 Mo3 C193 36.9(4) . . ? C213 Mo3 C193 136.8(5) . . ? C113 Mo3 C223 100.2(5) . . ? C213 Mo3 C223 36.3(4) . . ? C193 Mo3 C223 132.8(5) . . ? C113 Mo3 C293 132.0(5) . . ? C213 Mo3 C293 36.0(5) . . ? C193 Mo3 C293 155.4(4) . . ? C223 Mo3 C293 59.4(5) . . ? C113 Mo3 C123 35.8(4) . . ? C213 Mo3 C123 92.0(5) . . ? C193 Mo3 C123 59.7(4) . . ? C223 Mo3 C123 73.1(4) . . ? C293 Mo3 C123 127.5(5) . . ? C113 Mo3 C233 130.6(5) . . ? C213 Mo3 C233 58.2(4) . . ? C193 Mo3 C233 147.5(4) . . ? C223 Mo3 C233 35.4(4) . . ? C293 Mo3 C233 56.4(4) . . ? C123 Mo3 C233 96.5(4) . . ? C113 Mo3 C183 58.3(4) . . ? C213 Mo3 C183 148.5(5) . . ? C193 Mo3 C183 34.7(4) . . ? C223 Mo3 C183 118.5(4) . . ? C293 Mo3 C183 168.9(4) . . ? C123 Mo3 C183 57.0(4) . . ? C233 Mo3 C183 114.9(4) . . ? C113 Mo3 C133 58.0(4) . . ? C213 Mo3 C133 116.8(5) . . ? C193 Mo3 C133 57.8(4) . . ? C223 Mo3 C133 85.4(4) . . ? C293 Mo3 C133 143.6(4) . . ? C123 Mo3 C133 34.3(4) . . ? C233 Mo3 C133 90.0(4) . . ? C183 Mo3 C133 33.3(4) . . ? C113 Mo3 C283 156.4(4) . . ? C213 Mo3 C283 57.2(4) . . ? C193 Mo3 C283 166.0(4) . . ? C223 Mo3 C283 57.3(4) . . ? C293 Mo3 C283 33.3(4) . . ? C123 Mo3 C283 128.1(4) . . ? C233 Mo3 C283 32.7(4) . . ? C183 Mo3 C283 135.7(4) . . ? C133 Mo3 C283 120.6(4) . . ? C113 Mo3 Br23 124.7(4) . . ? C213 Mo3 Br23 129.6(4) . . ? C193 Mo3 Br23 88.2(3) . . ? C223 Mo3 Br23 133.1(3) . . ? C293 Mo3 Br23 93.6(4) . . ? C123 Mo3 Br23 137.3(3) . . ? C233 Mo3 Br23 98.2(3) . . ? C183 Mo3 Br23 80.4(3) . . ? C133 Mo3 Br23 105.9(3) . . ? C283 Mo3 Br23 78.9(3) . . ? C113 Mo3 Br13 80.3(3) . . ? C213 Mo3 Br13 85.8(3) . . ? C193 Mo3 Br13 78.6(3) . . ? C223 Mo3 Br13 121.7(3) . . ? C293 Mo3 Br13 77.3(3) . . ? C123 Mo3 Br13 114.3(3) . . ? C233 Mo3 Br13 133.7(3) . . ? C183 Mo3 Br13 110.9(3) . . ? C133 Mo3 Br13 134.7(3) . . ? C283 Mo3 Br13 104.7(3) . . ? Br23 Mo3 Br13 82.36(5) . . ? C123 C113 C193 107.8(11) . . ? C123 C113 Mo3 75.5(7) . . ? C193 C113 Mo3 72.4(7) . . ? C113 C123 C133 108.3(11) . . ? C113 C123 Mo3 68.7(6) . . ? C133 C123 Mo3 78.0(6) . . ? C143 C133 C183 119.5(10) . . ? C143 C133 C123 132.3(11) . . ? C183 C133 C123 108.2(10) . . ? C143 C133 Mo3 126.5(8) . . ? C183 C133 Mo3 73.4(6) . . ? C123 C133 Mo3 67.8(6) . . ? C153 C143 C133 119.3(13) . . ? C143 C153 C163 121.1(12) . . ? C173 C163 C153 123.4(13) . . ? C163 C173 C183 115.1(13) . . ? C133 C183 C173 121.4(11) . . ? C133 C183 C193 107.9(10) . . ? C173 C183 C193 130.7(12) . . ? C133 C183 Mo3 73.4(6) . . ? C173 C183 Mo3 128.5(8) . . ? C193 C183 Mo3 65.0(6) . . ? C183 C193 C113 107.6(11) . . ? C183 C193 Mo3 80.3(7) . . ? C113 C193 Mo3 70.7(7) . . ? C293 C213 C223 107.5(11) . . ? C293 C213 Mo3 74.0(7) . . ? C223 C213 Mo3 73.2(7) . . ? C213 C223 C233 106.4(11) . . ? C213 C223 Mo3 70.5(7) . . ? C233 C223 Mo3 78.2(7) . . ? C283 C233 C243 120.4(12) . . ? C283 C233 C223 109.3(10) . . ? C243 C233 C223 130.0(13) . . ? C283 C233 Mo3 77.6(7) . . ? C243 C233 Mo3 126.8(8) . . ? C223 C233 Mo3 66.4(6) . . ? C253 C243 C233 116.3(16) . . ? C243 C253 C263 124.0(18) . . ? C273 C263 C253 121.0(18) . . ? C263 C273 C283 119.2(17) . . ? C273 C283 C233 119.0(13) . . ? C273 C283 C293 135.1(14) . . ? C233 C283 C293 105.9(11) . . ? C273 C283 Mo3 130.6(9) . . ? C233 C283 Mo3 69.7(6) . . ? C293 C283 Mo3 63.9(6) . . ? C213 C293 C283 110.3(12) . . ? C213 C293 Mo3 70.0(7) . . ? C283 C293 Mo3 82.8(7) . . ? C114 Mo4 C294 136.8(5) . . ? C114 Mo4 C214 100.9(5) . . ? C294 Mo4 C214 36.6(4) . . ? C114 Mo4 C124 35.9(4) . . ? C294 Mo4 C124 132.4(5) . . ? C214 Mo4 C124 101.0(5) . . ? C114 Mo4 C194 36.6(4) . . ? C294 Mo4 C194 155.5(4) . . ? C214 Mo4 C194 131.6(4) . . ? C124 Mo4 C194 59.9(5) . . ? C114 Mo4 C224 90.1(5) . . ? C294 Mo4 C224 59.1(4) . . ? C214 Mo4 C224 34.7(4) . . ? C124 Mo4 C224 73.3(4) . . ? C194 Mo4 C224 126.5(5) . . ? C114 Mo4 C134 58.8(4) . . ? C294 Mo4 C134 146.2(4) . . ? C214 Mo4 C134 131.5(5) . . ? C124 Mo4 C134 35.6(4) . . ? C194 Mo4 C134 57.7(4) . . ? C224 Mo4 C134 97.8(4) . . ? C114 Mo4 C284 145.7(4) . . ? C294 Mo4 C284 35.1(3) . . ? C214 Mo4 C284 58.0(4) . . ? C124 Mo4 C284 116.1(4) . . ? C194 Mo4 C284 169.0(4) . . ? C224 Mo4 C284 56.7(4) . . ? C134 Mo4 C284 112.6(4) . . ? C114 Mo4 C234 114.1(4) . . ? C294 Mo4 C234 57.4(4) . . ? C214 Mo4 C234 57.3(4) . . ? C124 Mo4 C234 83.8(4) . . ? C194 Mo4 C234 143.0(4) . . ? C224 Mo4 C234 34.6(3) . . ? C134 Mo4 C234 89.4(4) . . ? C284 Mo4 C234 32.6(3) . . ? C114 Mo4 C184 57.5(4) . . ? C294 Mo4 C184 165.8(4) . . ? C214 Mo4 C184 156.9(4) . . ? C124 Mo4 C184 57.2(4) . . ? C194 Mo4 C184 33.8(4) . . ? C224 Mo4 C184 129.0(4) . . ? C134 Mo4 C184 33.1(4) . . ? C284 Mo4 C184 135.2(3) . . ? C234 Mo4 C184 121.0(4) . . ? C114 Mo4 Br24 86.4(3) . . ? C294 Mo4 Br24 79.9(3) . . ? C214 Mo4 Br24 80.4(3) . . ? C124 Mo4 Br24 122.1(3) . . ? C194 Mo4 Br24 76.3(3) . . ? C224 Mo4 Br24 112.7(3) . . ? C134 Mo4 Br24 133.9(3) . . ? C284 Mo4 Br24 113.0(3) . . ? C234 Mo4 Br24 134.9(3) . . ? C184 Mo4 Br24 104.0(3) . . ? C114 Mo4 Br14 131.3(4) . . ? C294 Mo4 Br14 87.4(3) . . ? C214 Mo4 Br14 123.4(3) . . ? C124 Mo4 Br14 133.3(3) . . ? C194 Mo4 Br14 94.8(4) . . ? C224 Mo4 Br14 137.8(3) . . ? C134 Mo4 Br14 98.0(3) . . ? C284 Mo4 Br14 81.0(3) . . ? C234 Mo4 Br14 107.0(2) . . ? C184 Mo4 Br14 79.6(3) . . ? Br24 Mo4 Br14 82.41(5) . . ? C224 C214 C294 108.7(10) . . ? C224 C214 Mo4 76.0(7) . . ? C294 C214 Mo4 71.4(6) . . ? C214 C224 C234 108.2(11) . . ? C214 C224 Mo4 69.3(7) . . ? C234 C224 Mo4 77.9(6) . . ? C284 C234 C244 120.3(9) . . ? C284 C234 C224 107.7(10) . . ? C244 C234 C224 132.0(11) . . ? C284 C234 Mo4 72.5(6) . . ? C244 C234 Mo4 126.9(8) . . ? C224 C234 Mo4 67.5(6) . . ? C254 C244 C234 116.4(11) . . ? C244 C254 C264 123.3(11) . . ? C274 C264 C254 121.5(10) . . ? C264 C274 C284 118.0(11) . . ? C234 C284 C274 120.3(10) . . ? C234 C284 C294 108.2(9) . . ? C274 C284 C294 131.6(11) . . ? C234 C284 Mo4 74.9(6) . . ? C274 C284 Mo4 126.9(7) . . ? C294 C284 Mo4 64.9(6) . . ? C214 C294 C284 107.0(11) . . ? C214 C294 Mo4 72.0(6) . . ? C284 C294 Mo4 80.1(6) . . ? C124 C114 C194 109.5(12) . . ? C124 C114 Mo4 74.7(7) . . ? C194 C114 Mo4 76.3(7) . . ? C184 C134 C144 119.6(12) . . ? C184 C134 C124 107.6(10) . . ? C144 C134 C124 132.4(12) . . ? C184 C134 Mo4 77.2(6) . . ? C144 C134 Mo4 127.5(8) . . ? C124 C134 Mo4 66.3(6) . . ? C154 C144 C134 117.5(13) . . ? C114 C124 C134 107.5(11) . . ? C114 C124 Mo4 69.3(7) . . ? C134 C124 Mo4 78.1(7) . . ? C144 C154 C164 122.1(13) . . ? C174 C164 C154 123.0(14) . . ? C164 C174 C184 116.8(13) . . ? C134 C184 C194 107.9(11) . . ? C134 C184 C174 120.4(11) . . ? C194 C184 C174 131.7(12) . . ? C134 C184 Mo4 69.7(6) . . ? C194 C184 Mo4 65.3(6) . . ? C174 C184 Mo4 130.1(8) . . ? C184 C194 C114 107.1(11) . . ? C184 C194 Mo4 80.9(6) . . ? C114 C194 Mo4 67.2(7) . . ? _diffrn_measured_fraction_theta_max 0.839 _diffrn_reflns_theta_full 26.13 _diffrn_measured_fraction_theta_full 0.839 _refine_diff_density_max 0.800 _refine_diff_density_min -0.774 _refine_diff_density_rms 0.192 #======END data_compound_6_[Ind2Mo{POMe3}2][PF6]2 _database_code_CSD 167780 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[Ind2Mo{POMe3}2][PF6]2' _chemical_formula_sum 'C24 H32 F12 Mo O6 P4' _chemical_formula_weight 864.32 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' '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' 'F' 'F' 0.0171 0.0103 '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/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 12.447(17) _cell_length_b 18.044(23) _cell_length_c 14.977(19) _cell_angle_alpha 90.00 _cell_angle_beta 99.99(1) _cell_angle_gamma 90.00 _cell_volume 3313(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.733 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 0.694 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11295 _diffrn_reflns_av_R_equivalents 0.0241 _diffrn_reflns_av_sigmaI/netI 0.0345 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.95 _reflns_number_total 6352 _reflns_number_gt 4839 _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 w==1/[\s^2^(Fo^2^)+(0.1225P)^2^+2.7157P] 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 SHELXL _refine_ls_extinction_coef 0.0069(9) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 6352 _refine_ls_number_parameters 431 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0853 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1910 _refine_ls_wR_factor_gt 0.1714 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.17930(3) 0.07686(2) 0.74028(2) 0.03768(19) Uani 1 d . . . P1 P 0.27199(12) -0.02982(7) 0.81934(9) 0.0461(3) Uani 1 d . . . O31 O 0.3474(4) -0.0708(2) 0.7614(3) 0.0639(11) Uani 1 d . . . C32 C 0.4005(7) -0.1414(4) 0.7793(5) 0.087(2) Uani 1 d . . . H32A H 0.4648 -0.1354 0.8245 0.104 Uiso 1 calc R . . H32B H 0.4207 -0.1601 0.7245 0.104 Uiso 1 calc R . . H32C H 0.3517 -0.1756 0.8007 0.104 Uiso 1 calc R . . O41 O 0.3448(3) -0.0090(2) 0.9126(3) 0.0592(10) Uani 1 d . . . C42 C 0.3965(7) -0.0631(4) 0.9795(5) 0.078(2) Uani 1 d . . . H42A H 0.3536 -0.1076 0.9747 0.094 Uiso 1 calc R . . H42B H 0.4014 -0.0427 1.0393 0.094 Uiso 1 calc R . . H42C H 0.4683 -0.0743 0.9682 0.094 Uiso 1 calc R . . O51 O 0.1967(3) -0.0968(2) 0.8406(3) 0.0570(9) Uani 1 d . . . C52 C 0.1249(6) -0.0898(4) 0.9067(5) 0.0711(17) Uani 1 d . . . H52A H 0.1631 -0.0657 0.9600 0.085 Uiso 1 calc R . . H52B H 0.1019 -0.1382 0.9224 0.085 Uiso 1 calc R . . H52C H 0.0622 -0.0609 0.8814 0.085 Uiso 1 calc R . . P2 P 0.35099(12) 0.10232(8) 0.68442(9) 0.0507(4) Uani 1 d . . . O61 O 0.3286(4) 0.1759(3) 0.6255(3) 0.0867(15) Uani 1 d . . . C62 C 0.3832(7) 0.2065(6) 0.5605(6) 0.105(3) Uani 1 d . . . H62A H 0.4506 0.1806 0.5610 0.126 Uiso 1 calc R . . H62B H 0.3979 0.2579 0.5739 0.126 Uiso 1 calc R . . H62C H 0.3385 0.2020 0.5016 0.126 Uiso 1 calc R . . O71 O 0.3954(4) 0.0470(3) 0.6204(3) 0.0777(13) Uani 1 d . . . C72 C 0.4919(6) 0.0046(5) 0.6341(6) 0.097(3) Uani 1 d . . . H72A H 0.5474 0.0303 0.6090 0.117 Uiso 1 calc R . . H72B H 0.4780 -0.0426 0.6046 0.117 Uiso 1 calc R . . H72C H 0.5162 -0.0029 0.6978 0.117 Uiso 1 calc R . . O81 O 0.4469(3) 0.1161(3) 0.7667(3) 0.0765(13) Uani 1 d . . . C82 C 0.5485(8) 0.1528(7) 0.7635(7) 0.138(4) Uani 1 d . . . H82A H 0.5655 0.1485 0.7036 0.165 Uiso 1 calc R . . H82B H 0.6054 0.1303 0.8063 0.165 Uiso 1 calc R . . H82C H 0.5425 0.2042 0.7784 0.165 Uiso 1 calc R . . C21 C 0.0503(5) -0.0090(3) 0.6872(4) 0.0609(15) Uani 1 d . . . H21 H 0.0271 -0.0418 0.7278 0.073 Uiso 1 calc R . . C22 C 0.0056(4) 0.0613(3) 0.6633(3) 0.0540(13) Uani 1 d . . . H22 H -0.0490 0.0843 0.6884 0.065 Uiso 1 calc R . . C23 C 0.0585(4) 0.0915(3) 0.5937(3) 0.0495(12) Uani 1 d . . . C24 C 0.0382(6) 0.1555(4) 0.5394(4) 0.0709(17) Uani 1 d . . . H24 H -0.0090 0.1921 0.5530 0.085 Uiso 1 calc R . . C25 C 0.0894(7) 0.1623(5) 0.4670(4) 0.091(2) Uani 1 d . . . H25 H 0.0754 0.2039 0.4301 0.109 Uiso 1 calc R . . C26 C 0.1631(7) 0.1084(6) 0.4458(4) 0.087(2) Uani 1 d . . . H26 H 0.1945 0.1144 0.3942 0.105 Uiso 1 calc R . . C27 C 0.1889(5) 0.0485(5) 0.4985(4) 0.0748(19) Uani 1 d . . . H27 H 0.2396 0.0143 0.4849 0.090 Uiso 1 calc R . . C28 C 0.1375(4) 0.0381(3) 0.5755(3) 0.0525(13) Uani 1 d . . . C29 C 0.1379(5) -0.0210(3) 0.6383(4) 0.0585(14) Uani 1 d . . . H29 H 0.1865 -0.0606 0.6462 0.070 Uiso 1 calc R . . C11 C 0.2639(5) 0.1430(3) 0.8606(3) 0.0520(13) Uani 1 d . . . H11 H 0.3377 0.1347 0.8817 0.062 Uiso 1 calc R . . C12 C 0.1753(5) 0.1053(3) 0.8904(3) 0.0548(13) Uani 1 d . . . H12 H 0.1815 0.0667 0.9322 0.066 Uiso 1 calc R . . C13 C 0.0774(5) 0.1367(3) 0.8458(3) 0.0504(12) Uani 1 d . . . C14 C -0.0337(6) 0.1264(4) 0.8578(4) 0.0723(18) Uani 1 d . . . H14 H -0.0529 0.0888 0.8946 0.087 Uiso 1 calc R . . C15 C -0.1107(6) 0.1743(5) 0.8126(6) 0.087(2) Uani 1 d . . . H15 H -0.1826 0.1703 0.8214 0.104 Uiso 1 calc R . . C16 C -0.0838(6) 0.2288(4) 0.7541(5) 0.079(2) Uani 1 d . . . H16 H -0.1391 0.2595 0.7250 0.094 Uiso 1 calc R . . C17 C 0.0198(6) 0.2395(3) 0.7372(4) 0.0648(16) Uani 1 d . . . H17 H 0.0349 0.2752 0.6963 0.078 Uiso 1 calc R . . C18 C 0.1035(4) 0.1935(3) 0.7852(3) 0.0459(11) Uani 1 d . . . C19 C 0.2198(5) 0.1954(3) 0.7929(3) 0.0511(13) Uani 1 d . . . H19 H 0.2593 0.2254 0.7597 0.061 Uiso 1 calc R . . P3 P 0.76596(15) -0.07899(10) 0.83454(11) 0.0640(4) Uani 1 d . . . F31 F 0.7268(9) -0.0096(4) 0.7827(6) 0.228(5) Uani 1 d . . . F32 F 0.8613(6) -0.0832(5) 0.7818(4) 0.173(4) Uani 1 d . . . F33 F 0.8369(5) -0.0322(3) 0.9113(3) 0.122(2) Uani 1 d . . . F34 F 0.6765(6) -0.0841(5) 0.8938(6) 0.183(4) Uani 1 d . . . F35 F 0.6956(5) -0.1267(4) 0.7579(4) 0.144(3) Uani 1 d . . . F36 F 0.8128(8) -0.1511(4) 0.8873(5) 0.179(3) Uani 1 d . . . P4 P 0.69907(15) 0.30210(9) 1.00327(12) 0.0665(5) Uani 1 d . . . F41 F 0.6275(11) 0.2445(6) 0.9559(7) 0.269(6) Uani 1 d . . . F42 F 0.6606(6) 0.2786(7) 1.0896(5) 0.207(4) Uani 1 d . . . F43 F 0.6098(7) 0.3569(5) 0.9797(9) 0.248(6) Uani 1 d . . . F44 F 0.7435(7) 0.3244(6) 0.9186(5) 0.195(4) Uani 1 d . . . F45 F 0.7943(7) 0.2482(5) 1.0327(7) 0.198(4) Uani 1 d . . . F46 F 0.7822(8) 0.3603(5) 1.0523(8) 0.217(4) Uani 1 d . . . 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 0.0472(3) 0.0338(3) 0.0315(3) -0.00053(15) 0.00523(17) -0.00205(16) P1 0.0559(8) 0.0353(6) 0.0456(7) 0.0030(5) 0.0048(6) -0.0016(5) O31 0.074(3) 0.050(2) 0.071(3) 0.0049(19) 0.023(2) 0.0155(18) C32 0.115(6) 0.056(4) 0.091(5) 0.008(4) 0.022(4) 0.035(4) O41 0.070(3) 0.047(2) 0.053(2) 0.0068(17) -0.0088(18) -0.0013(18) C42 0.101(5) 0.060(4) 0.064(4) 0.015(3) -0.014(4) 0.011(3) O51 0.069(2) 0.0391(18) 0.065(2) 0.0034(17) 0.0148(19) -0.0058(17) C52 0.069(4) 0.066(4) 0.082(4) 0.007(3) 0.022(3) -0.009(3) P2 0.0568(8) 0.0505(7) 0.0465(7) -0.0026(6) 0.0141(6) -0.0100(6) O61 0.107(4) 0.078(3) 0.083(3) 0.022(3) 0.040(3) -0.009(3) C62 0.086(5) 0.119(7) 0.110(6) 0.048(6) 0.017(5) -0.020(5) O71 0.061(3) 0.100(3) 0.074(3) -0.026(3) 0.017(2) 0.007(2) C72 0.080(5) 0.085(5) 0.130(7) -0.009(5) 0.027(5) 0.020(4) O81 0.057(2) 0.106(4) 0.066(3) -0.017(3) 0.009(2) -0.031(3) C82 0.107(7) 0.187(11) 0.118(7) -0.037(8) 0.016(6) -0.093(8) C21 0.061(3) 0.061(3) 0.055(3) 0.001(3) -0.006(3) -0.027(3) C22 0.042(3) 0.076(4) 0.042(3) -0.009(3) 0.001(2) -0.009(3) C23 0.052(3) 0.057(3) 0.036(2) -0.005(2) -0.003(2) -0.002(2) C24 0.085(5) 0.070(4) 0.051(3) 0.004(3) -0.008(3) 0.013(3) C25 0.114(6) 0.106(6) 0.046(3) 0.025(4) -0.004(4) -0.001(5) C26 0.093(5) 0.130(7) 0.038(3) 0.003(4) 0.008(3) -0.019(5) C27 0.067(4) 0.111(6) 0.046(3) -0.025(4) 0.007(3) -0.001(4) C28 0.052(3) 0.064(3) 0.039(2) -0.016(2) 0.002(2) -0.002(2) C29 0.076(4) 0.042(3) 0.052(3) -0.016(2) -0.004(3) 0.004(3) C11 0.060(3) 0.048(3) 0.044(3) -0.015(2) -0.003(2) 0.005(2) C12 0.084(4) 0.044(3) 0.037(2) -0.004(2) 0.012(3) 0.007(3) C13 0.069(3) 0.044(3) 0.041(2) -0.005(2) 0.019(2) 0.000(2) C14 0.080(4) 0.082(4) 0.065(4) -0.008(3) 0.041(3) -0.005(4) C15 0.061(4) 0.101(6) 0.104(6) -0.026(5) 0.031(4) 0.007(4) C16 0.075(5) 0.087(5) 0.073(4) -0.009(4) 0.010(4) 0.029(4) C17 0.084(4) 0.055(3) 0.055(3) -0.003(3) 0.008(3) 0.014(3) C18 0.060(3) 0.042(3) 0.037(2) 0.000(2) 0.011(2) 0.008(2) C19 0.075(4) 0.035(2) 0.047(3) -0.011(2) 0.021(3) -0.007(2) P3 0.0658(10) 0.0718(11) 0.0556(9) -0.0093(7) 0.0139(7) -0.0005(8) F31 0.295(12) 0.123(6) 0.215(8) 0.027(6) -0.102(9) 0.056(6) F32 0.110(4) 0.321(12) 0.100(4) -0.040(5) 0.052(3) -0.036(5) F33 0.157(5) 0.135(4) 0.070(3) -0.010(3) 0.011(3) -0.073(4) F34 0.119(5) 0.263(10) 0.189(7) -0.113(7) 0.086(5) -0.058(5) F35 0.138(5) 0.176(7) 0.114(4) -0.063(4) 0.008(4) -0.038(4) F36 0.257(9) 0.113(5) 0.159(6) 0.031(5) 0.016(6) 0.027(5) P4 0.0775(11) 0.0556(9) 0.0676(10) 0.0170(8) 0.0159(8) 0.0023(8) F41 0.359(15) 0.211(10) 0.198(9) -0.038(7) -0.062(9) -0.160(11) F42 0.170(7) 0.336(12) 0.134(5) 0.103(7) 0.082(5) 0.041(7) F43 0.163(7) 0.192(8) 0.407(15) 0.141(10) 0.101(8) 0.109(6) F44 0.182(7) 0.275(10) 0.142(6) 0.110(7) 0.065(5) 0.009(7) F45 0.171(7) 0.181(7) 0.259(9) 0.122(7) 0.083(7) 0.094(6) F46 0.191(8) 0.151(7) 0.291(12) -0.053(7) -0.008(8) -0.055(6) _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 C11 2.263(5) . ? Mo1 C21 2.272(5) . ? Mo1 C22 2.284(5) . ? Mo1 C19 2.305(5) . ? Mo1 C12 2.316(5) . ? Mo1 C29 2.334(5) . ? Mo1 P1 2.4422(13) . ? Mo1 C13 2.443(5) . ? Mo1 C18 2.449(5) . ? Mo1 C23 2.450(5) . ? Mo1 P2 2.4694(15) . ? Mo1 C28 2.531(5) . ? P1 O31 1.570(4) . ? P1 O41 1.573(4) . ? P1 O51 1.596(4) . ? O31 C32 1.438(7) . ? O41 C42 1.464(7) . ? O51 C52 1.449(7) . ? P2 O71 1.550(5) . ? P2 O81 1.580(4) . ? P2 O61 1.592(5) . ? O61 C62 1.394(8) . ? O71 C72 1.410(8) . ? O81 C82 1.436(9) . ? C21 C22 1.406(9) . ? C21 C29 1.432(9) . ? C22 C23 1.433(8) . ? C23 C24 1.411(8) . ? C23 C28 1.436(8) . ? C24 C25 1.354(10) . ? C25 C26 1.412(12) . ? C26 C27 1.344(12) . ? C27 C28 1.426(8) . ? C28 C29 1.421(8) . ? C11 C19 1.425(7) . ? C11 C12 1.432(8) . ? C12 C13 1.403(8) . ? C13 C14 1.437(8) . ? C13 C18 1.444(7) . ? C14 C15 1.379(11) . ? C15 C16 1.396(11) . ? C16 C17 1.371(10) . ? C17 C18 1.425(8) . ? C18 C19 1.432(8) . ? P3 F31 1.509(7) . ? P3 F32 1.538(6) . ? P3 F34 1.542(6) . ? P3 F33 1.569(5) . ? P3 F35 1.574(6) . ? P3 F36 1.581(7) . ? P4 F41 1.469(7) . ? P4 F43 1.483(7) . ? P4 F42 1.516(6) . ? P4 F44 1.522(6) . ? P4 F45 1.538(6) . ? P4 F46 1.564(8) . ? 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 C11 Mo1 C21 147.2(2) . . ? C11 Mo1 C22 137.4(2) . . ? C21 Mo1 C22 35.9(2) . . ? C11 Mo1 C19 36.34(19) . . ? C21 Mo1 C19 148.3(2) . . ? C22 Mo1 C19 114.7(2) . . ? C11 Mo1 C12 36.4(2) . . ? C21 Mo1 C12 111.0(2) . . ? C22 Mo1 C12 109.8(2) . . ? C19 Mo1 C12 60.16(19) . . ? C11 Mo1 C29 160.0(2) . . ? C21 Mo1 C29 36.2(2) . . ? C22 Mo1 C29 59.6(2) . . ? C19 Mo1 C29 159.5(2) . . ? C12 Mo1 C29 139.8(2) . . ? C11 Mo1 P1 85.08(14) . . ? C21 Mo1 P1 83.00(16) . . ? C22 Mo1 P1 118.30(16) . . ? C19 Mo1 P1 120.59(14) . . ? C12 Mo1 P1 77.99(14) . . ? C29 Mo1 P1 75.69(15) . . ? C11 Mo1 C13 58.3(2) . . ? C21 Mo1 C13 96.5(2) . . ? C22 Mo1 C13 80.13(19) . . ? C19 Mo1 C13 58.40(18) . . ? C12 Mo1 C13 34.17(19) . . ? C29 Mo1 C13 132.6(2) . . ? P1 Mo1 C13 106.81(13) . . ? C11 Mo1 C18 58.39(18) . . ? C21 Mo1 C18 113.6(2) . . ? C22 Mo1 C18 82.4(2) . . ? C19 Mo1 C18 34.89(18) . . ? C12 Mo1 C18 57.87(18) . . ? C29 Mo1 C18 141.2(2) . . ? P1 Mo1 C18 135.77(12) . . ? C13 Mo1 C18 34.34(16) . . ? C11 Mo1 C23 141.73(19) . . ? C21 Mo1 C23 58.2(2) . . ? C22 Mo1 C23 35.01(19) . . ? C19 Mo1 C23 105.68(19) . . ? C12 Mo1 C23 137.1(2) . . ? C29 Mo1 C23 57.56(19) . . ? P1 Mo1 C23 133.16(13) . . ? C13 Mo1 C23 103.02(19) . . ? C18 Mo1 C23 87.02(17) . . ? C11 Mo1 P2 82.01(16) . . ? C21 Mo1 P2 127.50(17) . . ? C22 Mo1 P2 130.60(14) . . ? C19 Mo1 P2 78.02(14) . . ? C12 Mo1 P2 116.97(16) . . ? C29 Mo1 P2 91.43(17) . . ? P1 Mo1 P2 86.97(5) . . ? C13 Mo1 P2 135.56(14) . . ? C18 Mo1 P2 109.29(13) . . ? C23 Mo1 P2 96.27(14) . . ? C11 Mo1 C28 155.6(2) . . ? C21 Mo1 C28 57.1(2) . . ? C22 Mo1 C28 57.12(18) . . ? C19 Mo1 C28 125.86(19) . . ? C12 Mo1 C28 166.6(2) . . ? C29 Mo1 C28 33.67(19) . . ? P1 Mo1 C28 104.76(14) . . ? C13 Mo1 C28 135.31(18) . . ? C18 Mo1 C28 118.81(17) . . ? C23 Mo1 C28 33.46(18) . . ? P2 Mo1 C28 76.40(13) . . ? O31 P1 O41 107.2(2) . . ? O31 P1 O51 100.4(2) . . ? O41 P1 O51 105.7(2) . . ? O31 P1 Mo1 112.38(16) . . ? O41 P1 Mo1 113.19(15) . . ? O51 P1 Mo1 116.73(16) . . ? C32 O31 P1 127.9(4) . . ? C42 O41 P1 124.5(4) . . ? C52 O51 P1 121.5(4) . . ? O71 P2 O81 106.4(3) . . ? O71 P2 O61 103.9(3) . . ? O81 P2 O61 109.7(3) . . ? O71 P2 Mo1 120.8(2) . . ? O81 P2 Mo1 110.24(17) . . ? O61 P2 Mo1 105.3(2) . . ? C62 O61 P2 131.1(6) . . ? C72 O71 P2 130.2(5) . . ? C82 O81 P2 126.6(5) . . ? C22 C21 C29 108.0(5) . . ? C22 C21 Mo1 72.5(3) . . ? C29 C21 Mo1 74.2(3) . . ? C21 C22 C23 108.5(5) . . ? C21 C22 Mo1 71.6(3) . . ? C23 C22 Mo1 78.8(3) . . ? C24 C23 C22 132.2(6) . . ? C24 C23 C28 120.0(5) . . ? C22 C23 C28 107.4(5) . . ? C24 C23 Mo1 128.7(4) . . ? C22 C23 Mo1 66.2(3) . . ? C28 C23 Mo1 76.4(3) . . ? C25 C24 C23 118.3(7) . . ? C24 C25 C26 122.1(7) . . ? C27 C26 C25 121.4(6) . . ? C26 C27 C28 119.1(7) . . ? C29 C28 C27 133.2(6) . . ? C29 C28 C23 107.6(5) . . ? C27 C28 C23 118.9(6) . . ? C29 C28 Mo1 65.5(3) . . ? C27 C28 Mo1 135.0(4) . . ? C23 C28 Mo1 70.2(3) . . ? C28 C29 C21 108.0(5) . . ? C28 C29 Mo1 80.8(3) . . ? C21 C29 Mo1 69.6(3) . . ? C19 C11 C12 108.3(5) . . ? C19 C11 Mo1 73.4(3) . . ? C12 C11 Mo1 73.8(3) . . ? C13 C12 C11 108.2(5) . . ? C13 C12 Mo1 77.9(3) . . ? C11 C12 Mo1 69.8(3) . . ? C12 C13 C14 131.5(5) . . ? C12 C13 C18 108.3(5) . . ? C14 C13 C18 119.8(5) . . ? C12 C13 Mo1 68.0(3) . . ? C14 C13 Mo1 130.0(4) . . ? C18 C13 Mo1 73.1(3) . . ? C15 C14 C13 117.3(6) . . ? C14 C15 C16 122.0(7) . . ? C17 C16 C15 123.4(7) . . ? C16 C17 C18 117.0(6) . . ? C17 C18 C19 131.8(5) . . ? C17 C18 C13 120.4(5) . . ? C19 C18 C13 107.5(4) . . ? C17 C18 Mo1 130.2(4) . . ? C19 C18 Mo1 67.1(3) . . ? C13 C18 Mo1 72.6(3) . . ? C11 C19 C18 107.5(5) . . ? C11 C19 Mo1 70.2(3) . . ? C18 C19 Mo1 78.1(3) . . ? F31 P3 F32 89.2(6) . . ? F31 P3 F34 98.3(6) . . ? F32 P3 F34 172.5(5) . . ? F31 P3 F33 91.2(4) . . ? F32 P3 F33 90.9(4) . . ? F34 P3 F33 88.9(3) . . ? F31 P3 F35 89.4(4) . . ? F32 P3 F35 88.9(4) . . ? F34 P3 F35 91.2(4) . . ? F33 P3 F35 179.4(4) . . ? F31 P3 F36 177.1(6) . . ? F32 P3 F36 88.0(5) . . ? F34 P3 F36 84.4(5) . . ? F33 P3 F36 88.0(4) . . ? F35 P3 F36 91.4(5) . . ? F41 P4 F43 89.4(7) . . ? F41 P4 F42 87.6(6) . . ? F43 P4 F42 93.1(5) . . ? F41 P4 F44 93.6(6) . . ? F43 P4 F44 89.5(5) . . ? F42 P4 F44 177.1(4) . . ? F41 P4 F45 93.6(7) . . ? F43 P4 F45 176.5(7) . . ? F42 P4 F45 85.4(5) . . ? F44 P4 F45 91.9(4) . . ? F41 P4 F46 176.1(7) . . ? F43 P4 F46 94.1(6) . . ? F42 P4 F46 93.9(6) . . ? F44 P4 F46 84.7(6) . . ? F45 P4 F46 82.9(6) . . ? _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 25.95 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 1.188 _refine_diff_density_min -0.636 _refine_diff_density_rms 0.140 #======END data_compound_8_[Ind2Mo(CO)Cl][BF4] _database_code_CSD 167781 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[Ind2Mo(CO)Cl][BF4]' _chemical_formula_sum 'C19 H14 B Cl F4 Mo O' _chemical_formula_weight 476.50 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' 'Mo' 'Mo' -1.6832 0.6857 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.897(14) _cell_length_b 9.332(14) _cell_length_c 12.334(17) _cell_angle_alpha 97.25(1) _cell_angle_beta 97.51(1) _cell_angle_gamma 113.11(1) _cell_volume 916(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_coefficient_mu 0.906 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3257 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1047 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 25.96 _reflns_number_total 3257 _reflns_number_gt 2145 _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 w==1/[\s^2^(Fo^2^)+(0.1227P)^2^+2.7175P] 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 3257 _refine_ls_number_parameters 242 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1684 _refine_ls_R_factor_gt 0.1053 _refine_ls_wR_factor_ref 0.2527 _refine_ls_wR_factor_gt 0.2240 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.71547(13) 0.81716(12) 0.76671(9) 0.0470(4) Uani 1 d . . . Cl1 Cl 0.8234(4) 0.6977(4) 0.9090(3) 0.0646(9) Uani 1 d . . . C100 C 0.9586(18) 0.9453(16) 0.7766(11) 0.062(3) Uani 1 d . . . O100 O 1.0958(13) 1.0235(13) 0.7818(9) 0.090(3) Uani 1 d . . . C11 C 0.729(2) 1.0658(15) 0.8097(11) 0.071(4) Uani 1 d . . . H11 H 0.8069 1.1480 0.7844 0.085 Uiso 1 calc R . . C12 C 0.7569(17) 1.0152(14) 0.9105(9) 0.057(3) Uani 1 d . . . H12 H 0.8580 1.0529 0.9605 0.069 Uiso 1 calc R . . C13 C 0.6001(16) 0.8939(15) 0.9223(10) 0.058(3) Uani 1 d . . . C14 C 0.5517(19) 0.8007(18) 1.0041(12) 0.073(4) Uani 1 d . . . H14 H 0.6299 0.8137 1.0668 0.088 Uiso 1 calc R . . C15 C 0.393(2) 0.693(2) 0.9920(16) 0.101(6) Uani 1 d . . . H15 H 0.3621 0.6302 1.0449 0.121 Uiso 1 calc R . . C16 C 0.273(2) 0.6771(19) 0.8966(15) 0.086(5) Uani 1 d . . . H16 H 0.1627 0.6052 0.8905 0.104 Uiso 1 calc R . . C17 C 0.3115(18) 0.761(2) 0.8152(14) 0.080(4) Uani 1 d . . . H17 H 0.2307 0.7491 0.7543 0.096 Uiso 1 calc R . . C18 C 0.4824(16) 0.8708(15) 0.8261(11) 0.058(3) Uani 1 d . . . C19 C 0.5636(19) 0.9709(15) 0.7538(11) 0.064(4) Uani 1 d . . . H19 H 0.5158 0.9730 0.6826 0.077 Uiso 1 calc R . . C21 C 0.7376(15) 0.7807(15) 0.5857(9) 0.056(3) Uani 1 d . . . H21 H 0.8065 0.8646 0.5569 0.067 Uiso 1 calc R . . C22 C 0.7860(16) 0.6749(15) 0.6355(11) 0.057(3) Uani 1 d . . . H22 H 0.8947 0.6836 0.6512 0.068 Uiso 1 calc R . . C23 C 0.6445(14) 0.5520(13) 0.6586(10) 0.047(3) Uani 1 d . . . C24 C 0.6167(17) 0.4110(14) 0.7037(10) 0.057(3) Uani 1 d . . . H24 H 0.7040 0.3834 0.7262 0.068 Uiso 1 calc R . . C25 C 0.4592(19) 0.3201(16) 0.7120(12) 0.068(4) Uani 1 d . . . H25 H 0.4392 0.2267 0.7387 0.081 Uiso 1 calc R . . C26 C 0.3208(17) 0.3593(16) 0.6820(11) 0.069(4) Uani 1 d . . . H26 H 0.2152 0.2916 0.6898 0.083 Uiso 1 calc R . . C27 C 0.3416(15) 0.4952(14) 0.6420(10) 0.055(3) Uani 1 d . . . H217 H 0.2524 0.5218 0.6236 0.065 Uiso 1 calc R . . C28 C 0.5045(14) 0.5933(14) 0.6300(9) 0.049(3) Uani 1 d . . . C29 C 0.5659(16) 0.7391(15) 0.5862(9) 0.055(3) Uani 1 d . . . H29 H 0.5045 0.7944 0.5630 0.066 Uiso 1 calc R . . B1 B 0.8415(14) 1.2045(16) 0.5298(13) 0.091(7) Uani 1 d D . . F11 F 0.6882(17) 1.124(2) 0.5483(17) 0.094(7) Uiso 0.59(2) d PD . . F12 F 0.854(2) 1.287(2) 0.4457(14) 0.097(6) Uiso 0.59(2) d PD . . F13 F 0.9426(18) 1.1293(18) 0.5287(15) 0.099(6) Uiso 0.59(2) d PD . . F14 F 0.919(2) 1.325(2) 0.6319(17) 0.150(10) Uiso 0.59(2) d PD . . F21 F 0.6747(19) 1.093(2) 0.512(2) 0.080(8) Uiso 0.41(2) d PD . . F22 F 0.844(3) 1.345(2) 0.513(3) 0.114(10) Uiso 0.41(2) d PD . . F23 F 0.894(4) 1.138(4) 0.440(2) 0.20(2) Uiso 0.41(2) d PD . . F24 F 0.930(3) 1.199(3) 0.6239(18) 0.121(11) Uiso 0.41(2) d PD . . 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 0.0420(6) 0.0431(6) 0.0470(6) 0.0077(4) 0.0085(4) 0.0089(4) Cl1 0.065(2) 0.0588(19) 0.0575(18) 0.0135(15) -0.0026(15) 0.0171(16) C100 0.061(9) 0.058(8) 0.062(8) 0.027(7) 0.003(7) 0.016(7) O100 0.059(7) 0.078(7) 0.097(8) 0.020(6) 0.014(6) -0.009(6) C11 0.104(12) 0.041(7) 0.058(8) 0.005(6) 0.033(8) 0.016(8) C12 0.069(9) 0.045(7) 0.043(6) -0.008(5) 0.020(6) 0.011(6) C13 0.062(8) 0.052(7) 0.048(7) -0.008(6) 0.017(6) 0.017(6) C14 0.074(10) 0.077(10) 0.060(8) 0.007(7) 0.020(7) 0.023(8) C15 0.084(13) 0.099(13) 0.096(13) 0.013(11) 0.052(11) 0.005(10) C16 0.060(10) 0.076(10) 0.093(12) -0.019(9) 0.028(9) 0.003(8) C17 0.048(8) 0.101(12) 0.086(11) -0.011(9) 0.008(7) 0.035(8) C18 0.056(8) 0.052(7) 0.066(8) 0.003(6) 0.004(6) 0.027(6) C19 0.091(11) 0.051(8) 0.057(8) 0.001(6) 0.009(7) 0.042(8) C21 0.051(8) 0.058(8) 0.045(6) 0.014(6) 0.014(5) 0.006(6) C22 0.047(7) 0.056(8) 0.072(8) 0.023(7) 0.016(6) 0.022(6) C23 0.038(6) 0.043(6) 0.054(7) 0.001(5) 0.002(5) 0.015(5) C24 0.062(8) 0.047(7) 0.061(8) 0.010(6) 0.017(6) 0.021(7) C25 0.086(11) 0.044(7) 0.068(9) 0.013(6) 0.015(8) 0.021(7) C26 0.058(9) 0.054(8) 0.068(9) -0.002(7) 0.017(7) -0.003(7) C27 0.042(7) 0.050(7) 0.063(8) -0.001(6) 0.006(6) 0.016(6) C28 0.051(7) 0.058(7) 0.033(5) -0.003(5) 0.019(5) 0.020(6) C29 0.067(9) 0.055(7) 0.043(6) 0.010(5) 0.006(6) 0.028(7) B1 0.032(8) 0.101(14) 0.17(2) 0.104(15) 0.044(11) 0.034(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 C100 1.997(15) . ? Mo1 C21 2.262(11) . ? Mo1 C11 2.265(13) . ? Mo1 C22 2.270(13) . ? Mo1 C12 2.272(11) . ? Mo1 C29 2.305(12) . ? Mo1 C19 2.330(12) . ? Mo1 C28 2.436(12) . ? Mo1 C13 2.448(11) . ? Mo1 C23 2.453(11) . ? Mo1 Cl1 2.478(3) . ? Mo1 C18 2.491(12) . ? C100 O100 1.138(15) . ? C11 C19 1.41(2) . ? C11 C12 1.411(18) . ? C12 C13 1.451(17) . ? C13 C18 1.408(18) . ? C13 C14 1.415(18) . ? C14 C15 1.35(2) . ? C15 C16 1.43(3) . ? C16 C17 1.35(2) . ? C17 C18 1.438(19) . ? C18 C19 1.428(19) . ? C21 C22 1.399(17) . ? C21 C29 1.422(17) . ? C22 C23 1.423(16) . ? C23 C24 1.438(16) . ? C23 C28 1.456(16) . ? C24 C25 1.350(18) . ? C25 C26 1.43(2) . ? C26 C27 1.372(18) . ? C27 C28 1.418(16) . ? C28 C29 1.456(16) . ? B1 F24 1.333(17) . ? B1 F11 1.339(15) . ? B1 F13 1.341(14) . ? B1 F22 1.342(17) . ? B1 F12 1.359(14) . ? B1 F21 1.408(16) . ? B1 F23 1.419(17) . ? B1 F14 1.459(17) . ? F12 F22 0.97(3) . ? F12 F23 1.57(3) . ? F13 F23 1.14(3) . ? F13 F24 1.31(3) . ? F14 F24 1.21(3) . ? F14 F22 1.59(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C100 Mo1 C21 78.3(5) . . ? C100 Mo1 C11 79.7(6) . . ? C21 Mo1 C11 106.0(5) . . ? C100 Mo1 C22 75.7(5) . . ? C21 Mo1 C22 36.0(4) . . ? C11 Mo1 C22 138.1(4) . . ? C100 Mo1 C12 81.4(5) . . ? C21 Mo1 C12 140.2(4) . . ? C11 Mo1 C12 36.2(5) . . ? C22 Mo1 C12 157.0(5) . . ? C100 Mo1 C29 112.8(5) . . ? C21 Mo1 C29 36.3(4) . . ? C11 Mo1 C29 100.5(5) . . ? C22 Mo1 C29 60.2(4) . . ? C12 Mo1 C29 133.7(5) . . ? C100 Mo1 C19 112.0(5) . . ? C21 Mo1 C19 97.4(5) . . ? C11 Mo1 C19 35.7(5) . . ? C22 Mo1 C19 132.3(5) . . ? C12 Mo1 C19 59.6(5) . . ? C29 Mo1 C19 74.5(5) . . ? C100 Mo1 C28 133.0(5) . . ? C21 Mo1 C28 58.8(4) . . ? C11 Mo1 C28 127.6(5) . . ? C22 Mo1 C28 58.5(4) . . ? C12 Mo1 C28 144.4(4) . . ? C29 Mo1 C28 35.6(4) . . ? C19 Mo1 C28 93.2(5) . . ? C100 Mo1 C13 115.2(5) . . ? C21 Mo1 C13 154.2(5) . . ? C11 Mo1 C13 58.6(4) . . ? C22 Mo1 C13 163.1(4) . . ? C12 Mo1 C13 35.5(4) . . ? C29 Mo1 C13 121.3(5) . . ? C19 Mo1 C13 57.7(5) . . ? C28 Mo1 C13 111.8(4) . . ? C100 Mo1 C23 107.4(5) . . ? C21 Mo1 C23 58.5(4) . . ? C11 Mo1 C23 159.6(5) . . ? C22 Mo1 C23 34.8(4) . . ? C12 Mo1 C23 161.2(4) . . ? C29 Mo1 C23 59.1(4) . . ? C19 Mo1 C23 127.7(4) . . ? C28 Mo1 C23 34.6(4) . . ? C13 Mo1 C23 129.3(4) . . ? C100 Mo1 Cl1 81.9(4) . . ? C21 Mo1 Cl1 124.1(4) . . ? C11 Mo1 Cl1 121.1(4) . . ? C22 Mo1 Cl1 88.5(3) . . ? C12 Mo1 Cl1 85.9(4) . . ? C29 Mo1 Cl1 138.1(3) . . ? C19 Mo1 Cl1 138.4(3) . . ? C28 Mo1 Cl1 105.4(3) . . ? C13 Mo1 Cl1 80.8(3) . . ? C23 Mo1 Cl1 79.2(3) . . ? C100 Mo1 C18 135.4(5) . . ? C21 Mo1 C18 122.0(5) . . ? C11 Mo1 C18 57.3(5) . . ? C22 Mo1 C18 144.9(5) . . ? C12 Mo1 C18 57.4(5) . . ? C29 Mo1 C18 88.4(4) . . ? C19 Mo1 C18 34.3(4) . . ? C28 Mo1 C18 87.1(4) . . ? C13 Mo1 C18 33.1(4) . . ? C23 Mo1 C18 117.1(4) . . ? Cl1 Mo1 C18 108.7(3) . . ? O100 C100 Mo1 177.2(12) . . ? C19 C11 C12 108.5(12) . . ? C19 C11 Mo1 74.7(7) . . ? C12 C11 Mo1 72.1(7) . . ? C11 C12 C13 107.9(12) . . ? C11 C12 Mo1 71.6(7) . . ? C13 C12 Mo1 78.9(6) . . ? C18 C13 C14 119.6(13) . . ? C18 C13 C12 106.7(11) . . ? C14 C13 C12 133.7(13) . . ? C18 C13 Mo1 75.1(7) . . ? C14 C13 Mo1 123.1(10) . . ? C12 C13 Mo1 65.6(6) . . ? C15 C14 C13 120.4(15) . . ? C14 C15 C16 119.3(16) . . ? C17 C16 C15 123.0(15) . . ? C16 C17 C18 117.5(15) . . ? C13 C18 C19 108.9(12) . . ? C13 C18 C17 120.0(13) . . ? C19 C18 C17 131.1(13) . . ? C13 C18 Mo1 71.8(7) . . ? C19 C18 Mo1 66.7(7) . . ? C17 C18 Mo1 128.4(9) . . ? C11 C19 C18 107.7(12) . . ? C11 C19 Mo1 69.7(8) . . ? C18 C19 Mo1 79.0(7) . . ? C22 C21 C29 108.9(10) . . ? C22 C21 Mo1 72.3(7) . . ? C29 C21 Mo1 73.5(7) . . ? C21 C22 C23 110.0(10) . . ? C21 C22 Mo1 71.7(7) . . ? C23 C22 Mo1 79.7(7) . . ? C22 C23 C24 135.0(11) . . ? C22 C23 C28 106.2(10) . . ? C24 C23 C28 118.8(10) . . ? C22 C23 Mo1 65.5(7) . . ? C24 C23 Mo1 125.8(8) . . ? C28 C23 Mo1 72.0(6) . . ? C25 C24 C23 117.5(12) . . ? C24 C25 C26 123.7(12) . . ? C27 C26 C25 121.2(12) . . ? C26 C27 C28 117.3(12) . . ? C27 C28 C23 121.6(11) . . ? C27 C28 C29 130.8(11) . . ? C23 C28 C29 107.6(10) . . ? C27 C28 Mo1 127.1(8) . . ? C23 C28 Mo1 73.3(6) . . ? C29 C28 Mo1 67.3(6) . . ? C21 C29 C28 106.9(10) . . ? C21 C29 Mo1 70.2(7) . . ? C28 C29 Mo1 77.1(6) . . ? F24 B1 F11 98.8(15) . . ? F24 B1 F13 58.6(12) . . ? F11 B1 F13 117.4(12) . . ? F24 B1 F22 119(2) . . ? F11 B1 F22 104.1(15) . . ? F13 B1 F22 138.4(15) . . ? F24 B1 F12 141.8(16) . . ? F11 B1 F12 116.9(12) . . ? F13 B1 F12 110.6(12) . . ? F22 B1 F12 42.0(12) . . ? F24 B1 F21 111.0(14) . . ? F11 B1 F21 19.7(13) . . ? F13 B1 F21 109.7(14) . . ? F22 B1 F21 108.9(13) . . ? F12 B1 F21 107.1(14) . . ? F24 B1 F23 107.0(14) . . ? F11 B1 F23 118.8(18) . . ? F13 B1 F23 48.9(14) . . ? F22 B1 F23 109.5(14) . . ? F12 B1 F23 68.5(15) . . ? F21 B1 F23 99.7(14) . . ? F24 B1 F14 51.0(14) . . ? F11 B1 F14 101.8(13) . . ? F13 B1 F14 102.4(12) . . ? F22 B1 F14 69.1(16) . . ? F12 B1 F14 105.3(15) . . ? F21 B1 F14 121.5(15) . . ? F23 B1 F14 137.5(17) . . ? F22 F12 B1 68.1(13) . . ? F22 F12 F23 124.1(18) . . ? B1 F12 F23 57.5(10) . . ? F23 F13 F24 128.8(16) . . ? F23 F13 B1 69.1(12) . . ? F24 F13 B1 60.4(10) . . ? F24 F14 B1 59.1(10) . . ? F24 F14 F22 110.1(14) . . ? B1 F14 F22 52.0(9) . . ? F12 F22 B1 70.0(12) . . ? F12 F22 F14 120(2) . . ? B1 F22 F14 58.9(12) . . ? F13 F23 B1 62.0(10) . . ? F13 F23 F12 109.0(16) . . ? B1 F23 F12 53.9(9) . . ? F14 F24 F13 120(2) . . ? F14 F24 B1 69.9(14) . . ? F13 F24 B1 61.0(10) . . ? _diffrn_measured_fraction_theta_max 0.909 _diffrn_reflns_theta_full 25.96 _diffrn_measured_fraction_theta_full 0.909 _refine_diff_density_max 0.974 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.138 #======END