# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 #TrackingRef '- archive.cif' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2011-09-23 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? #------------------ AUTHOR DETAILS -------------------------------------------# # Name and address of author for correspondence _publ_contact_author_name 'Gallucci, Judith C.' _publ_contact_author_address ;Department of Chemistry The Ohio State University 100 West 18th Avenue Columbus, OH 43210 USA ; _publ_contact_author_email gallucci.1@osu.edu _publ_requested_category FM loop_ _publ_author_name 'Samantha Brown-Xu' 'Malcolm Chisholm' 'Judith Gallucci' 'Yagnaseni Ghosh' 'Terry Gustafson' 'Carly Reed' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_Chisholm1755 _database_code_depnum_ccdc_archive 'CCDC 849730' #TrackingRef '- archive.cif' _audit_creation_date 2011-09-23T16:58:01-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common 'Chisholm 1755' _chemical_formula_moiety 'C42 H52 Mo2 O8 Se2, 4(C4 H8 O)' _chemical_formula_sum 'C58 H84 Mo2 O12 Se2' _chemical_formula_weight 1323.05 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I41/a _symmetry_space_group_name_Hall '-I 4ad' _symmetry_Int_Tables_number 88 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 28.6622(2) _cell_length_b 28.6622(2) _cell_length_c 14.9089(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 12248.03(15) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7295 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description chunk _exptl_crystal_colour orange _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.31 _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5440 _exptl_special_details ;All work was done at 150 K using an Oxford Cryosystems Cryostream Cooler. The data collection strategy was set up to measure a quadrant of reciprocal space with a redundancy factor of 4.5, which means that 90% of these reflections were measured at least 4.5 times. Phi and omega scans with a frame width of 1.0 degree were used. Data integration was done with Denzo, and scaling and merging of the data was done with Scalepack. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.654 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.563 _exptl_absorpt_correction_T_max 0.599 _exptl_absorpt_process_details 'HKL Scalepack (Otwinowski & Minor, 1997)' #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.343701E-1 _diffrn_orient_matrix_ub_12 0.48575E-2 _diffrn_orient_matrix_ub_13 0.67567E-2 _diffrn_orient_matrix_ub_21 0.41782E-2 _diffrn_orient_matrix_ub_22 -0.47372E-2 _diffrn_orient_matrix_ub_23 -0.659656E-1 _diffrn_orient_matrix_ub_31 -0.43001E-2 _diffrn_orient_matrix_ub_32 0.342229E-1 _diffrn_orient_matrix_ub_33 -0.01009 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_av_unetI/netI ? _diffrn_reflns_number 122942 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.1 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 7018 _reflns_number_gt 5490 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ;The Mo dimer contains a crystallographic inversion center. There is a THF molecule located on each end of this dimer with the oxygen atom of the THF positioned to interact with the Mo atom. This THF molecule contains some disorder, with atoms C(23) and C(24) disordered over two sites: C(23A), C(24A) and C(23B), C(24B). A SADI restraint for these two bond lengths was applied during the least-squares refinement. Atoms C(23B) and C(24B) were kept isotropic. There is also a solvent molecule of THF in the asymmetric unit. For each methyl group, the hydrogen atoms were added at calculated positions using a riding model with U(H) = 1.5 * Ueq(bonded carbon atom). The rest of the hydrogen atoms were included in the model at calculated positions using a riding model with U(H) = 1.2 * Ueq(bonded atom). 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^ > 2\s(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 'w=1/[\s^2^(Fo^2^)+(0.0442P)^2^+15.9436P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7018 _refine_ls_number_parameters 343 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0505 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0861 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.588 _refine_diff_density_min -0.461 _refine_diff_density_rms 0.069 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Mo Mo 0.465770(7) 0.513005(7) 0.003969(13) 0.02094(7) Uani 1 1 d . . . Se Se 0.608948(10) 0.620820(10) 0.17720(2) 0.04165(9) Uani 1 1 d . . . O1 O 0.47598(6) 0.55422(5) -0.11224(11) 0.0254(4) Uani 1 1 d . . . O2 O 0.48601(5) 0.56994(6) 0.08314(11) 0.0259(4) Uani 1 1 d . . . O3 O 0.44079(6) 0.45685(6) -0.07474(11) 0.0259(4) Uani 1 1 d . . . O4 O 0.45178(6) 0.47458(6) 0.12103(11) 0.0261(4) Uani 1 1 d . . . O5 O 0.38045(6) 0.53964(7) -0.01691(14) 0.0416(5) Uani 1 1 d . A . C1 C 0.51533(8) 0.55077(8) -0.15126(16) 0.0257(5) Uani 1 1 d . . . C2 C 0.52319(9) 0.57677(9) -0.23715(17) 0.0284(5) Uani 1 1 d . . . C3 C 0.49995(10) 0.56161(10) -0.31484(17) 0.0342(6) Uani 1 1 d . . . C4 C 0.50848(10) 0.58518(10) -0.39455(18) 0.0380(6) Uani 1 1 d . . . H4 H 0.493 0.5753 -0.4476 0.046 Uiso 1 1 calc R . . C5 C 0.53868(10) 0.62252(10) -0.39907(18) 0.0371(6) Uani 1 1 d . . . C6 C 0.56121(10) 0.63711(9) -0.32136(19) 0.0372(6) Uani 1 1 d . . . H6 H 0.5818 0.6631 -0.3241 0.045 Uiso 1 1 calc R . . C7 C 0.55432(9) 0.61444(9) -0.23890(18) 0.0315(6) Uani 1 1 d . . . C8 C 0.46868(11) 0.51862(11) -0.3135(2) 0.0446(7) Uani 1 1 d . . . H8 H 0.4571 0.5148 -0.2507 0.053 Uiso 1 1 calc R . . C9 C 0.49607(16) 0.47530(12) -0.3367(3) 0.0793(13) Uani 1 1 d . . . H9A H 0.4753 0.4482 -0.3357 0.119 Uiso 1 1 calc R . . H9B H 0.5211 0.4709 -0.2928 0.119 Uiso 1 1 calc R . . H9C H 0.5096 0.4787 -0.3967 0.119 Uiso 1 1 calc R . . C10 C 0.42623(15) 0.52294(16) -0.3737(4) 0.0920(15) Uani 1 1 d . . . H10A H 0.4077 0.4943 -0.37 0.138 Uiso 1 1 calc R . . H10B H 0.4363 0.5278 -0.4358 0.138 Uiso 1 1 calc R . . H10C H 0.4072 0.5495 -0.3542 0.138 Uiso 1 1 calc R . . C11 C 0.54770(12) 0.64656(11) -0.4888(2) 0.0476(8) Uani 1 1 d . . . H11 H 0.5271 0.6315 -0.5344 0.057 Uiso 1 1 calc R . . C12 C 0.53597(16) 0.69749(12) -0.4869(2) 0.0693(11) Uani 1 1 d . . . H12A H 0.5034 0.7015 -0.4687 0.104 Uiso 1 1 calc R . . H12B H 0.5405 0.7108 -0.5468 0.104 Uiso 1 1 calc R . . H12C H 0.5564 0.7135 -0.4441 0.104 Uiso 1 1 calc R . . C13 C 0.59753(17) 0.6392(2) -0.5182(3) 0.127(3) Uani 1 1 d . . . H13A H 0.6045 0.6057 -0.5192 0.191 Uiso 1 1 calc R . . H13B H 0.6186 0.6549 -0.4761 0.191 Uiso 1 1 calc R . . H13C H 0.6019 0.6522 -0.5784 0.191 Uiso 1 1 calc R . . C14 C 0.57828(10) 0.63083(10) -0.1532(2) 0.0382(6) Uani 1 1 d . . . H14 H 0.5843 0.6026 -0.1156 0.046 Uiso 1 1 calc R . . C15 C 0.54700(13) 0.66274(14) -0.0997(3) 0.0664(11) Uani 1 1 d . . . H15A H 0.5632 0.6727 -0.0451 0.1 Uiso 1 1 calc R . . H15B H 0.5184 0.6461 -0.0834 0.1 Uiso 1 1 calc R . . H15C H 0.5391 0.6902 -0.1359 0.1 Uiso 1 1 calc R . . C16 C 0.62531(12) 0.65459(17) -0.1695(3) 0.0776(12) Uani 1 1 d . . . H16A H 0.6456 0.6337 -0.204 0.116 Uiso 1 1 calc R . . H16B H 0.64 0.6618 -0.1118 0.116 Uiso 1 1 calc R . . H16C H 0.6204 0.6836 -0.2032 0.116 Uiso 1 1 calc R . . C17 C 0.52940(8) 0.57319(8) 0.10116(16) 0.0254(5) Uani 1 1 d . . . C18 C 0.54568(9) 0.61331(9) 0.15302(17) 0.0281(5) Uani 1 1 d . . . C19 C 0.51965(10) 0.64854(9) 0.18841(19) 0.0365(6) Uani 1 1 d . . . H19 H 0.4867 0.6502 0.182 0.044 Uiso 1 1 calc R . . C20 C 0.54610(11) 0.68272(10) 0.2359(2) 0.0426(7) Uani 1 1 d . . . H20 H 0.5321 0.709 0.2641 0.051 Uiso 1 1 calc R . . C21 C 0.59246(11) 0.67483(10) 0.2376(2) 0.0431(7) Uani 1 1 d . . . H21 H 0.6143 0.6948 0.2665 0.052 Uiso 1 1 calc R . . C22 C 0.36204(11) 0.54760(13) -0.1041(3) 0.0582(9) Uani 1 1 d . . . H22A H 0.3876 0.5528 -0.1476 0.07 Uiso 0.598(9) 1 calc PR A 1 H22B H 0.3416 0.5754 -0.104 0.07 Uiso 0.598(9) 1 calc PR A 1 H22C H 0.3763 0.5255 -0.1472 0.07 Uiso 0.402(9) 1 calc PR A 2 H22D H 0.3696 0.5797 -0.1237 0.07 Uiso 0.402(9) 1 calc PR A 2 C23A C 0.3359(3) 0.5068(2) -0.1282(5) 0.070(2) Uani 0.598(9) 1 d PD A 1 H23A H 0.3548 0.486 -0.1669 0.084 Uiso 0.598(9) 1 calc PR A 1 H23B H 0.3071 0.5156 -0.1609 0.084 Uiso 0.598(9) 1 calc PR A 1 C24A C 0.3244(3) 0.4836(3) -0.0435(5) 0.075(2) Uani 0.598(9) 1 d PD A 1 H24A H 0.3368 0.4514 -0.043 0.091 Uiso 0.598(9) 1 calc PR A 1 H24B H 0.2902 0.4823 -0.0352 0.091 Uiso 0.598(9) 1 calc PR A 1 C23B C 0.3118(5) 0.5413(5) -0.1031(9) 0.097(5) Uiso 0.402(9) 1 d PD A 2 H23C H 0.2955 0.5716 -0.0974 0.116 Uiso 0.402(9) 1 calc PR A 2 H23D H 0.301 0.5254 -0.1583 0.116 Uiso 0.402(9) 1 calc PR A 2 C24B C 0.3044(7) 0.5126(8) -0.0252(11) 0.139(7) Uiso 0.402(9) 1 d PD A 2 H24C H 0.2966 0.4804 -0.044 0.167 Uiso 0.402(9) 1 calc PR A 2 H24D H 0.278 0.525 0.0102 0.167 Uiso 0.402(9) 1 calc PR A 2 C25 C 0.34652(12) 0.51210(15) 0.0299(3) 0.0645(10) Uani 1 1 d . . . H25A H 0.3232 0.5321 0.06 0.077 Uiso 0.598(9) 1 calc PR A 1 H25B H 0.3616 0.4918 0.0751 0.077 Uiso 0.598(9) 1 calc PR A 1 H25C H 0.3401 0.5256 0.0897 0.077 Uiso 0.402(9) 1 calc PR A 2 H25D H 0.3579 0.4798 0.0378 0.077 Uiso 0.402(9) 1 calc PR A 2 O1A O 0.2192(2) 0.4224(2) 0.0123(4) 0.163(2) Uani 1 1 d . . . C1A C 0.2514(3) 0.38440(17) 0.0406(4) 0.115(2) Uani 1 1 d . . . H1A1 H 0.2468 0.356 0.0039 0.138 Uiso 1 1 calc R . . H1A2 H 0.2844 0.3944 0.0361 0.138 Uiso 1 1 calc R . . C2A C 0.2381(2) 0.3765(2) 0.1328(4) 0.1118(18) Uani 1 1 d . . . H2A1 H 0.266 0.3696 0.1697 0.134 Uiso 1 1 calc R . . H2A2 H 0.2163 0.3498 0.137 0.134 Uiso 1 1 calc R . . C3A C 0.2156(4) 0.4192(4) 0.1638(6) 0.184(5) Uani 1 1 d . . . H3A1 H 0.1887 0.4121 0.2033 0.221 Uiso 1 1 calc R . . H3A2 H 0.2378 0.4393 0.1967 0.221 Uiso 1 1 calc R . . C4A C 0.2015(3) 0.4397(4) 0.0874(8) 0.201(5) Uani 1 1 d . . . H4A1 H 0.167 0.4373 0.084 0.241 Uiso 1 1 calc R . . H4A2 H 0.2095 0.4732 0.0906 0.241 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 Mo 0.02066(11) 0.02118(11) 0.02097(11) 0.00006(8) -0.00042(8) 0.00055(7) Se 0.03148(15) 0.04328(17) 0.05020(19) -0.01565(14) -0.00116(13) -0.00743(12) O1 0.0261(9) 0.0258(8) 0.0241(9) 0.0034(7) 0.0008(7) 0.0022(7) O2 0.0241(9) 0.0250(8) 0.0285(9) -0.0039(7) -0.0014(7) 0.0024(7) O3 0.0241(8) 0.0257(8) 0.0280(9) -0.0032(7) -0.0029(7) -0.0005(7) O4 0.0262(9) 0.0274(9) 0.0249(9) 0.0036(7) 0.0015(7) 0.0015(7) O5 0.0279(10) 0.0422(11) 0.0546(13) -0.0026(9) -0.0022(9) 0.0022(8) C1 0.0304(13) 0.0250(12) 0.0217(12) -0.0002(10) 0.0001(10) -0.0023(10) C2 0.0306(13) 0.0284(13) 0.0263(13) 0.0042(10) 0.0050(10) 0.0042(10) C3 0.0380(15) 0.0384(15) 0.0261(13) 0.0005(11) 0.0010(11) 0.0018(11) C4 0.0474(17) 0.0409(16) 0.0256(14) 0.0006(12) 0.0007(12) 0.0058(13) C5 0.0452(16) 0.0379(15) 0.0280(14) 0.0070(12) 0.0071(12) 0.0112(13) C6 0.0365(15) 0.0322(14) 0.0428(16) 0.0084(12) 0.0087(13) 0.0030(11) C7 0.0314(13) 0.0297(13) 0.0332(14) 0.0049(11) 0.0041(11) 0.0040(11) C8 0.0560(19) 0.0489(18) 0.0288(14) -0.0020(13) -0.0034(13) -0.0118(14) C9 0.089(3) 0.043(2) 0.106(4) -0.005(2) 0.003(3) -0.011(2) C10 0.074(3) 0.078(3) 0.125(4) 0.013(3) -0.044(3) -0.028(2) C11 0.064(2) 0.0476(18) 0.0310(16) 0.0114(13) 0.0077(14) 0.0072(15) C12 0.115(3) 0.049(2) 0.044(2) 0.0179(16) 0.005(2) 0.001(2) C13 0.098(4) 0.207(6) 0.077(3) 0.088(4) 0.057(3) 0.071(4) C14 0.0391(15) 0.0344(15) 0.0411(16) 0.0078(12) -0.0046(13) -0.0056(12) C15 0.055(2) 0.089(3) 0.055(2) -0.028(2) -0.0070(18) -0.0025(19) C16 0.044(2) 0.117(4) 0.072(3) -0.006(2) -0.0055(19) -0.022(2) C17 0.0294(13) 0.0240(12) 0.0228(12) 0.0014(10) 0.0003(10) -0.0020(10) C18 0.0307(13) 0.0271(13) 0.0265(13) -0.0020(10) -0.0022(10) -0.0047(10) C19 0.0406(15) 0.0331(14) 0.0357(15) -0.0067(12) -0.0035(12) -0.0029(12) C20 0.0503(18) 0.0339(15) 0.0438(17) -0.0133(13) 0.0017(14) -0.0052(13) C21 0.0480(18) 0.0384(16) 0.0428(17) -0.0132(13) 0.0026(13) -0.0137(13) C22 0.0385(17) 0.071(2) 0.066(2) 0.0167(19) -0.0138(16) 0.0029(16) C23A 0.078(5) 0.058(4) 0.075(5) -0.006(3) -0.037(4) -0.007(3) C24A 0.068(5) 0.061(4) 0.097(6) 0.000(4) 0.001(4) -0.038(4) C25 0.0386(18) 0.084(3) 0.071(2) 0.011(2) 0.0132(17) 0.0037(18) O1A 0.179(5) 0.159(5) 0.150(5) 0.049(4) -0.016(4) 0.008(4) C1A 0.207(7) 0.062(3) 0.077(4) 0.000(3) -0.003(4) 0.001(4) C2A 0.110(4) 0.128(5) 0.097(4) 0.013(4) 0.016(3) 0.008(4) C3A 0.219(10) 0.216(10) 0.118(6) -0.068(7) 0.068(7) -0.064(8) C4A 0.189(9) 0.226(11) 0.187(10) -0.049(9) 0.072(8) 0.102(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 Mo O2 2.0959(16) . ? Mo O4 2.1023(16) . ? Mo Mo 2.1024(4) 9_665 ? Mo O3 2.1166(16) . ? Mo O1 2.1173(16) . ? Se C21 1.852(3) . ? Se C18 1.861(2) . ? O1 C1 1.273(3) . ? O2 C17 1.276(3) . ? O3 C17 1.275(3) 9_665 ? O4 C1 1.273(3) 9_665 ? O5 C22 1.422(4) . ? O5 C25 1.434(4) . ? C1 O4 1.273(3) 9_665 ? C1 C2 1.499(3) . ? C2 C7 1.401(4) . ? C2 C3 1.405(4) . ? C3 C4 1.389(4) . ? C3 C8 1.524(4) . ? C4 C5 1.378(4) . ? C4 H4 0.95 . ? C5 C6 1.391(4) . ? C5 C11 1.527(4) . ? C6 C7 1.405(4) . ? C6 H6 0.95 . ? C7 C14 1.525(4) . ? C8 C9 1.509(5) . ? C8 C10 1.517(5) . ? C8 H8 1 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 C12 1.498(5) . ? C11 C13 1.509(5) . ? C11 H11 1 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 C15 1.509(5) . ? C14 C16 1.530(4) . ? C14 H14 1 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 O3 1.275(3) 9_665 ? C17 C18 1.462(3) . ? C18 C19 1.362(4) . ? C19 C20 1.427(4) . ? C19 H19 0.95 . ? C20 C21 1.348(4) . ? C20 H20 0.95 . ? C21 H21 0.95 . ? C22 C23A 1.433(7) . ? C22 C23B 1.450(13) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C22 H22C 0.99 . ? C22 H22D 0.99 . ? C23A C24A 1.464(8) . ? C23A H23A 0.99 . ? C23A H23B 0.99 . ? C24A C25 1.505(8) . ? C24A H24A 0.99 . ? C24A H24B 0.99 . ? C23B C24B 1.439(11) . ? C23B H23C 0.99 . ? C23B H23D 0.99 . ? C24B C25 1.459(18) . ? C24B H24C 0.99 . ? C24B H24D 0.99 . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C25 H25C 0.99 . ? C25 H25D 0.99 . ? O1A C4A 1.327(8) . ? O1A C1A 1.489(7) . ? C1A C2A 1.443(7) . ? C1A H1A1 0.99 . ? C1A H1A2 0.99 . ? C2A C3A 1.459(10) . ? C2A H2A1 0.99 . ? C2A H2A2 0.99 . ? C3A C4A 1.344(11) . ? C3A H3A1 0.99 . ? C3A H3A2 0.99 . ? C4A H4A1 0.99 . ? C4A H4A2 0.99 . ? 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 O2 Mo O4 89.61(6) . . ? O2 Mo Mo 92.83(4) . 9_665 ? O4 Mo Mo 92.24(5) . 9_665 ? O2 Mo O3 176.29(6) . . ? O4 Mo O3 89.85(6) . . ? Mo Mo O3 90.85(4) 9_665 . ? O2 Mo O1 89.32(6) . . ? O4 Mo O1 176.35(6) . . ? Mo Mo O1 91.30(4) 9_665 . ? O3 Mo O1 90.99(6) . . ? C21 Se C18 86.69(12) . . ? C1 O1 Mo 116.95(15) . . ? C17 O2 Mo 116.44(15) . . ? C17 O3 Mo 117.25(15) 9_665 . ? C1 O4 Mo 116.85(15) 9_665 . ? C22 O5 C25 106.3(3) . . ? O1 C1 O4 122.6(2) . 9_665 ? O1 C1 C2 119.0(2) . . ? O4 C1 C2 118.4(2) 9_665 . ? C7 C2 C3 121.7(2) . . ? C7 C2 C1 119.7(2) . . ? C3 C2 C1 118.6(2) . . ? C4 C3 C2 118.1(3) . . ? C4 C3 C8 120.5(2) . . ? C2 C3 C8 121.2(2) . . ? C5 C4 C3 122.0(3) . . ? C5 C4 H4 119 . . ? C3 C4 H4 119 . . ? C4 C5 C6 119.0(3) . . ? C4 C5 C11 120.0(3) . . ? C6 C5 C11 121.0(3) . . ? C5 C6 C7 121.7(3) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C2 C7 C6 117.5(3) . . ? C2 C7 C14 120.6(2) . . ? C6 C7 C14 121.9(2) . . ? C9 C8 C10 110.4(3) . . ? C9 C8 C3 110.9(3) . . ? C10 C8 C3 113.5(3) . . ? C9 C8 H8 107.3 . . ? C10 C8 H8 107.3 . . ? C3 C8 H8 107.3 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C13 110.7(4) . . ? C12 C11 C5 112.7(3) . . ? C13 C11 C5 110.6(3) . . ? C12 C11 H11 107.5 . . ? C13 C11 H11 107.5 . . ? C5 C11 H11 107.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C7 111.2(2) . . ? C15 C14 C16 109.7(3) . . ? C7 C14 C16 113.6(3) . . ? C15 C14 H14 107.3 . . ? C7 C14 H14 107.3 . . ? C16 C14 H14 107.3 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O3 C17 O2 122.6(2) 9_665 . ? O3 C17 C18 118.7(2) 9_665 . ? O2 C17 C18 118.7(2) . . ? C19 C18 C17 127.8(2) . . ? C19 C18 Se 111.90(19) . . ? C17 C18 Se 120.27(18) . . ? C18 C19 C20 114.2(3) . . ? C18 C19 H19 122.9 . . ? C20 C19 H19 122.9 . . ? C21 C20 C19 114.7(3) . . ? C21 C20 H20 122.7 . . ? C19 C20 H20 122.7 . . ? C20 C21 Se 112.5(2) . . ? C20 C21 H21 123.8 . . ? Se C21 H21 123.8 . . ? O5 C22 C23A 107.0(4) . . ? O5 C22 C23B 109.8(6) . . ? O5 C22 H22A 110.3 . . ? C23A C22 H22A 110.3 . . ? O5 C22 H22B 110.3 . . ? C23A C22 H22B 110.3 . . ? H22A C22 H22B 108.6 . . ? O5 C22 H22C 109.7 . . ? C23B C22 H22C 109.7 . . ? O5 C22 H22D 109.7 . . ? C23B C22 H22D 109.7 . . ? H22C C22 H22D 108.2 . . ? C22 C23A C24A 105.8(5) . . ? C22 C23A H23A 110.6 . . ? C24A C23A H23A 110.6 . . ? C22 C23A H23B 110.6 . . ? C24A C23A H23B 110.6 . . ? H23A C23A H23B 108.7 . . ? C23A C24A C25 106.6(4) . . ? C23A C24A H24A 110.4 . . ? C25 C24A H24A 110.4 . . ? C23A C24A H24B 110.4 . . ? C25 C24A H24B 110.4 . . ? H24A C24A H24B 108.6 . . ? C24B C23B C22 103.1(11) . . ? C24B C23B H23C 111.2 . . ? C22 C23B H23C 111.2 . . ? C24B C23B H23D 111.2 . . ? C22 C23B H23D 111.2 . . ? H23C C23B H23D 109.1 . . ? C23B C24B C25 109.7(13) . . ? C23B C24B H24C 109.7 . . ? C25 C24B H24C 109.7 . . ? C23B C24B H24D 109.7 . . ? C25 C24B H24D 109.7 . . ? H24C C24B H24D 108.2 . . ? O5 C25 C24B 106.4(6) . . ? O5 C25 C24A 103.3(4) . . ? O5 C25 H25A 111.1 . . ? C24A C25 H25A 111.1 . . ? O5 C25 H25B 111.1 . . ? C24A C25 H25B 111.1 . . ? H25A C25 H25B 109.1 . . ? O5 C25 H25C 110.5 . . ? C24B C25 H25C 110.5 . . ? O5 C25 H25D 110.5 . . ? C24B C25 H25D 110.5 . . ? H25C C25 H25D 108.6 . . ? C4A O1A C1A 105.7(6) . . ? C2A C1A O1A 102.8(5) . . ? C2A C1A H1A1 111.2 . . ? O1A C1A H1A1 111.2 . . ? C2A C1A H1A2 111.2 . . ? O1A C1A H1A2 111.2 . . ? H1A1 C1A H1A2 109.1 . . ? C1A C2A C3A 106.7(6) . . ? C1A C2A H2A1 110.4 . . ? C3A C2A H2A1 110.4 . . ? C1A C2A H2A2 110.4 . . ? C3A C2A H2A2 110.4 . . ? H2A1 C2A H2A2 108.6 . . ? C4A C3A C2A 103.3(7) . . ? C4A C3A H3A1 111.1 . . ? C2A C3A H3A1 111.1 . . ? C4A C3A H3A2 111.1 . . ? C2A C3A H3A2 111.1 . . ? H3A1 C3A H3A2 109.1 . . ? O1A C4A C3A 116.0(8) . . ? O1A C4A H4A1 108.3 . . ? C3A C4A H4A1 108.3 . . ? O1A C4A H4A2 108.3 . . ? C3A C4A H4A2 108.3 . . ? H4A1 C4A H4A2 107.4 . . ? 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 O2 Mo O1 C1 95.01(17) . . . . ? O4 Mo O1 C1 168.0(10) . . . . ? Mo Mo O1 C1 2.20(16) 9_665 . . . ? O3 Mo O1 C1 -88.68(17) . . . . ? O4 Mo O2 C17 93.36(17) . . . . ? Mo Mo O2 C17 1.14(16) 9_665 . . . ? O3 Mo O2 C17 175.0(9) . . . . ? O1 Mo O2 C17 -90.13(17) . . . . ? O2 Mo O3 C17 -173.7(9) . . . 9_665 ? O4 Mo O3 C17 -92.04(17) . . . 9_665 ? Mo Mo O3 C17 0.19(16) 9_665 . . 9_665 ? O1 Mo O3 C17 91.51(17) . . . 9_665 ? O2 Mo O4 C1 -92.77(16) . . . 9_665 ? Mo Mo O4 C1 0.05(16) 9_665 . . 9_665 ? O3 Mo O4 C1 90.90(16) . . . 9_665 ? O1 Mo O4 C1 -165.8(10) . . . 9_665 ? Mo O1 C1 O4 -2.8(3) . . . 9_665 ? Mo O1 C1 C2 175.99(16) . . . . ? O1 C1 C2 C7 111.1(3) . . . . ? O4 C1 C2 C7 -70.1(3) 9_665 . . . ? O1 C1 C2 C3 -70.8(3) . . . . ? O4 C1 C2 C3 108.0(3) 9_665 . . . ? C7 C2 C3 C4 -0.2(4) . . . . ? C1 C2 C3 C4 -178.3(2) . . . . ? C7 C2 C3 C8 175.9(3) . . . . ? C1 C2 C3 C8 -2.2(4) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C8 C3 C4 C5 -176.2(3) . . . . ? C3 C4 C5 C6 -0.1(4) . . . . ? C3 C4 C5 C11 178.6(3) . . . . ? C4 C5 C6 C7 0.7(4) . . . . ? C11 C5 C6 C7 -178.1(3) . . . . ? C3 C2 C7 C6 0.7(4) . . . . ? C1 C2 C7 C6 178.8(2) . . . . ? C3 C2 C7 C14 178.7(2) . . . . ? C1 C2 C7 C14 -3.3(4) . . . . ? C5 C6 C7 C2 -1.0(4) . . . . ? C5 C6 C7 C14 -178.9(3) . . . . ? C4 C3 C8 C9 85.1(4) . . . . ? C2 C3 C8 C9 -90.9(4) . . . . ? C4 C3 C8 C10 -39.8(4) . . . . ? C2 C3 C8 C10 144.2(3) . . . . ? C4 C5 C11 C12 121.9(3) . . . . ? C6 C5 C11 C12 -59.4(4) . . . . ? C4 C5 C11 C13 -113.6(4) . . . . ? C6 C5 C11 C13 65.2(4) . . . . ? C2 C7 C14 C15 -82.5(3) . . . . ? C6 C7 C14 C15 95.4(3) . . . . ? C2 C7 C14 C16 153.1(3) . . . . ? C6 C7 C14 C16 -29.0(4) . . . . ? Mo O2 C17 O3 -1.6(3) . . . 9_665 ? Mo O2 C17 C18 177.49(16) . . . . ? O3 C17 C18 C19 -178.8(3) 9_665 . . . ? O2 C17 C18 C19 2.1(4) . . . . ? O3 C17 C18 Se 1.5(3) 9_665 . . . ? O2 C17 C18 Se -177.61(17) . . . . ? C21 Se C18 C19 0.2(2) . . . . ? C21 Se C18 C17 179.9(2) . . . . ? C17 C18 C19 C20 179.9(3) . . . . ? Se C18 C19 C20 -0.4(3) . . . . ? C18 C19 C20 C21 0.4(4) . . . . ? C19 C20 C21 Se -0.3(4) . . . . ? C18 Se C21 C20 0.1(2) . . . . ? C25 O5 C22 C23A -33.7(5) . . . . ? C25 O5 C22 C23B 21.1(7) . . . . ? O5 C22 C23A C24A 21.4(7) . . . . ? C23B C22 C23A C24A -80.8(8) . . . . ? C22 C23A C24A C25 -1.9(8) . . . . ? O5 C22 C23B C24B -21.6(14) . . . . ? C23A C22 C23B C24B 74.8(12) . . . . ? C22 C23B C24B C25 14.0(18) . . . . ? C22 O5 C25 C24B -11.5(11) . . . . ? C22 O5 C25 C24A 31.1(5) . . . . ? C23B C24B C25 O5 -1.9(18) . . . . ? C23B C24B C25 C24A -93.6(17) . . . . ? C23A C24A C25 O5 -17.7(7) . . . . ? C23A C24A C25 C24B 82.0(10) . . . . ? C4A O1A C1A C2A 15.0(8) . . . . ? O1A C1A C2A C3A -22.7(8) . . . . ? C1A C2A C3A C4A 22.3(11) . . . . ? C1A O1A C4A C3A -1.1(13) . . . . ? C2A C3A C4A O1A -13.2(14) . . . . ? # END of CIF