Supplementary material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _journal_volume ? _journal_year 2001 _journal_page_first 2762 _publ_requested_journal 'J.Chem.Soc.,Dalton Trans. (0186)' loop_ _publ_author_name 'Seisenbaeva, Gulaim A.' 'Shevelkov, Andrei V.' 'Tegenfeldt, J.' 'Kloo, Lars' 'Drobot, Dmitrii V.' 'Kessler, Vadim G.' _publ_contact_author_name 'Dr Vadim G Kessler' _publ_contact_author_address ; Dr Vadim G Kessler Department of Chemistry SLU PO Box 7015 SE-750 07 Uppsala SWEDEN ; _publ_contact_author_email 'Vadim.Kessler@kemi.slu.se' #Compound 1 data_reomem _database_code_CSD 152226 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H36 O18 Re4' _chemical_formula_weight 1213.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Re' 'Re' -1.0185 7.2310 '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' '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' _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 7.8993(8) _cell_length_b 15.994(2) _cell_length_c 17.501(1) _cell_angle_alpha 113.434(2) _cell_angle_beta 93.048(2) _cell_angle_gamma 92.736(2) _cell_volume 2020.1(6) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 999 (I>10sigma(I)) _cell_measurement_theta_min 1.39 _cell_measurement_theta_max 28.28 _exptl_crystal_description prism _exptl_crystal_colour reddish black _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.960 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 17.799 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.0460 _exptl_absorpt_correction_T_max 0.0624 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12007 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0745 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 28.28 _reflns_number_total 8746 _reflns_number_gt 5990 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0256P)^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 0.000325(18) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8746 _refine_ls_number_parameters 479 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0701 _refine_ls_wR_factor_gt 0.0664 _refine_ls_goodness_of_fit_ref 0.832 _refine_ls_restrained_S_all 0.832 _refine_ls_shift/su_max 0.144 _refine_ls_shift/su_mean 0.002 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 Re1 Re 0.41991(5) 0.16099(3) 0.04948(3) 0.03178(11) Uani 1 1 d . . . Re2 Re 0.36326(5) -0.04495(3) -0.14787(2) 0.03092(11) Uani 1 1 d . . . Re3 Re 0.19812(5) 0.31247(3) 0.79540(2) 0.02868(10) Uani 1 1 d . . . Re4 Re -0.01065(5) 0.46234(2) 0.73358(2) 0.02876(10) Uani 1 1 d . . . Re5 Re 0.10074(5) 0.33101(3) 0.51690(2) 0.03027(11) Uani 1 1 d . . . Re6 Re 0.30294(5) 0.17974(3) 0.57972(2) 0.03107(11) Uani 1 1 d . . . O1 O 0.4302(7) 0.0551(4) -0.0483(4) 0.0290(15) Uani 1 1 d . . . O2 O 0.3372(8) 0.2968(4) 0.5603(4) 0.0334(16) Uani 1 1 d . . . O3 O 0.0820(9) 0.3990(4) 0.6308(4) 0.0349(17) Uani 1 1 d . . . O4 O 0.2302(8) 0.4351(4) 0.7826(4) 0.0333(16) Uani 1 1 d . . . O5 O -0.0424(8) 0.3468(4) 0.7572(4) 0.0342(17) Uani 1 1 d . . . O6 O 0.0651(8) 0.2075(4) 0.5273(4) 0.0359(17) Uani 1 1 d . . . O7 O 0.3896(8) 0.0877(4) 0.1226(4) 0.0332(16) Uani 1 1 d . . . O8 O -0.0556(9) 0.5228(4) 0.8472(4) 0.0425(19) Uani 1 1 d . . . O9 O 0.2045(8) 0.2434(4) 0.6811(4) 0.0306(16) Uani 1 1 d . . . O10 O 0.1410(9) 0.3806(4) 0.9067(4) 0.0398(18) Uani 1 1 d . . . O11 O 0.1711(9) 0.2665(4) 0.4079(4) 0.0407(18) Uani 1 1 d . . . O12 O 0.3366(8) -0.1272(4) -0.0836(4) 0.0365(17) Uani 1 1 d . . . O13 O 0.3458(8) -0.1563(4) -0.2434(4) 0.0396(17) Uani 1 1 d . . . O14 O 0.3509(9) 0.1211(4) 0.4658(4) 0.0436(19) Uani 1 1 d . . . O15 O 0.0864(9) 0.2095(4) 0.8050(4) 0.0359(17) Uani 1 1 d . . . O16 O 0.2138(9) 0.4352(4) 0.5119(4) 0.0395(18) Uani 1 1 d . . . O17 O 0.4059(9) 0.3112(5) 0.8178(4) 0.0446(19) Uani 1 1 d . . . O18 O 0.0853(9) 0.5772(4) 0.7440(4) 0.0384(17) Uani 1 1 d . . . O19 O -0.2095(9) 0.4541(5) 0.6917(5) 0.048(2) Uani 1 1 d . . . O20 O 0.4558(9) 0.2704(4) 0.1504(4) 0.0467(19) Uani 1 1 d . . . O21 O 0.5267(9) 0.2283(4) -0.0037(4) 0.0405(18) Uani 1 1 d . . . O22 O -0.1051(9) 0.3310(4) 0.4886(4) 0.0443(19) Uani 1 1 d . . . O23 O 0.1592(8) -0.0211(5) -0.1470(4) 0.0454(19) Uani 1 1 d . . . O24 O 0.2030(9) 0.0656(4) 0.5672(4) 0.047(2) Uani 1 1 d . . . O25 O 0.2087(9) 0.1664(5) 0.0365(4) 0.0418(18) Uani 1 1 d . . . O26 O 0.4983(9) 0.1874(5) 0.6239(5) 0.052(2) Uani 1 1 d . . . O27 O 0.4594(9) 0.0075(4) -0.2163(4) 0.0425(18) Uani 1 1 d . . . C1 C 0.3911(12) 0.4636(7) 0.7618(6) 0.040(3) Uani 1 1 d . . . H1A H 0.4822 0.4506 0.7929 0.060 Uiso 1 1 calc R . . H1B H 0.3962 0.5277 0.7750 0.060 Uiso 1 1 calc R . . H1C H 0.4017 0.4312 0.7035 0.060 Uiso 1 1 calc R . . C2 C -0.0999(12) 0.1826(7) 0.5508(7) 0.042(3) Uani 1 1 d . . . H2A H -0.1225 0.2278 0.6036 0.063 Uiso 1 1 calc R . . H2B H -0.0966 0.1245 0.5543 0.063 Uiso 1 1 calc R . . H2C H -0.1882 0.1793 0.5097 0.063 Uiso 1 1 calc R . . C3 C 0.4979(13) 0.3169(7) 0.5322(7) 0.052(3) Uani 1 1 d . . . H3A H 0.5896 0.2999 0.5600 0.078 Uiso 1 1 calc R . . H3B H 0.5128 0.3808 0.5448 0.078 Uiso 1 1 calc R . . H3C H 0.4974 0.2831 0.4734 0.078 Uiso 1 1 calc R . . C4 C -0.1986(13) 0.3293(7) 0.7896(7) 0.049(3) Uani 1 1 d . . . H4A H -0.2024 0.3731 0.8455 0.073 Uiso 1 1 calc R . . H4B H -0.2028 0.2692 0.7891 0.073 Uiso 1 1 calc R . . H4C H -0.2942 0.3341 0.7558 0.073 Uiso 1 1 calc R . . C5 C 0.2377(13) 0.0291(7) 0.1095(7) 0.048(3) Uani 1 1 d . . . H5A H 0.1431 0.0552 0.0929 0.073 Uiso 1 1 calc R . . H5B H 0.2169 0.0224 0.1600 0.073 Uiso 1 1 calc R . . H5C H 0.2517 -0.0294 0.0667 0.073 Uiso 1 1 calc R . . C6 C 0.5183(15) 0.1026(7) -0.1921(7) 0.052(3) Uani 1 1 d . . . H6A H 0.4484 0.1288 -0.2219 0.078 Uiso 1 1 calc R . . H6B H 0.6342 0.1065 -0.2048 0.078 Uiso 1 1 calc R . . H6C H 0.5110 0.1352 -0.1336 0.078 Uiso 1 1 calc R . . C7 C 0.1890(13) -0.1927(7) -0.1050(7) 0.049(3) Uani 1 1 d . . . H7A H 0.0872 -0.1620 -0.1039 0.073 Uiso 1 1 calc R . . H7B H 0.1868 -0.2203 -0.0656 0.073 Uiso 1 1 calc R . . H7C H 0.1958 -0.2388 -0.1596 0.073 Uiso 1 1 calc R . . C8 C 0.1091(14) 0.1804(7) 0.3490(6) 0.046(3) Uani 1 1 d . . . H8A H 0.0855 0.1406 0.3764 0.069 Uiso 1 1 calc R . . H8B H 0.1928 0.1558 0.3103 0.069 Uiso 1 1 calc R . . H8C H 0.0067 0.1859 0.3199 0.069 Uiso 1 1 calc R . . C9 C 0.1670(15) 0.6009(7) 0.6835(7) 0.057(3) Uani 1 1 d . . . H9A H 0.2021 0.5469 0.6410 0.086 Uiso 1 1 calc R . . H9B H 0.2647 0.6425 0.7100 0.086 Uiso 1 1 calc R . . H9C H 0.0888 0.6291 0.6591 0.086 Uiso 1 1 calc R . . C10 C 0.3694(14) 0.0275(7) 0.4170(6) 0.051(3) Uani 1 1 d . . . H10A H 0.4865 0.0153 0.4212 0.076 Uiso 1 1 calc R . . H10B H 0.3329 0.0137 0.3601 0.076 Uiso 1 1 calc R . . H10C H 0.3011 -0.0096 0.4368 0.076 Uiso 1 1 calc R . . C11 C 0.2141(14) 0.4692(7) 0.9585(6) 0.046(3) Uani 1 1 d . . . H11A H 0.3341 0.4671 0.9687 0.069 Uiso 1 1 calc R . . H11B H 0.1625 0.4905 1.0102 0.069 Uiso 1 1 calc R . . H11C H 0.1949 0.5099 0.9315 0.069 Uiso 1 1 calc R . . C12 C 0.2673(15) 0.4491(7) 0.4413(7) 0.054(3) Uani 1 1 d . . . H12A H 0.2065 0.4050 0.3918 0.082 Uiso 1 1 calc R . . H12B H 0.3871 0.4424 0.4381 0.082 Uiso 1 1 calc R . . H12C H 0.2442 0.5092 0.4465 0.082 Uiso 1 1 calc R . . C13 C 0.1253(16) 0.0422(7) 0.6291(7) 0.060(4) Uani 1 1 d . . . H13A H 0.2064 0.0156 0.6537 0.090 Uiso 1 1 calc R . . H13B H 0.0288 -0.0006 0.6036 0.090 Uiso 1 1 calc R . . H13C H 0.0891 0.0961 0.6713 0.090 Uiso 1 1 calc R . . C14 C 0.3791(15) -0.1716(7) -0.3249(6) 0.053(3) Uani 1 1 d . . . H14A H 0.3400 -0.1229 -0.3381 0.080 Uiso 1 1 calc R . . H14B H 0.3210 -0.2282 -0.3623 0.080 Uiso 1 1 calc R . . H14C H 0.4993 -0.1743 -0.3300 0.080 Uiso 1 1 calc R . . C15 C 0.0455(15) 0.1982(8) 0.8780(7) 0.055(3) Uani 1 1 d . . . H15A H 0.1441 0.2156 0.9170 0.083 Uiso 1 1 calc R . . H15B H 0.0092 0.1356 0.8643 0.083 Uiso 1 1 calc R . . H15C H -0.0443 0.2358 0.9022 0.083 Uiso 1 1 calc R . . C16 C 0.3748(15) 0.2896(7) 0.2239(7) 0.050(3) Uani 1 1 d . . . H16A H 0.2559 0.2707 0.2104 0.076 Uiso 1 1 calc R . . H16B H 0.3887 0.3538 0.2571 0.076 Uiso 1 1 calc R . . H16C H 0.4246 0.2574 0.2543 0.076 Uiso 1 1 calc R . . C17 C -0.0813(16) 0.6162(6) 0.8929(7) 0.056(4) Uani 1 1 d . . . H17A H 0.0186 0.6532 0.8939 0.084 Uiso 1 1 calc R . . H17B H -0.1032 0.6257 0.9487 0.084 Uiso 1 1 calc R . . H17C H -0.1768 0.6328 0.8671 0.084 Uiso 1 1 calc R . . C18 C 0.5626(17) 0.3252(7) 0.0242(8) 0.073(4) Uani 1 1 d . . . H18A H 0.4906 0.3561 0.0672 0.110 Uiso 1 1 calc R . . H18B H 0.5417 0.3427 -0.0214 0.110 Uiso 1 1 calc R . . H18C H 0.6795 0.3412 0.0456 0.110 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 Re1 0.0412(3) 0.0251(2) 0.0303(2) 0.01098(18) 0.00959(19) 0.00779(18) Re2 0.0361(2) 0.0278(2) 0.0287(2) 0.01086(18) 0.00437(18) 0.00298(18) Re3 0.0366(2) 0.0250(2) 0.0268(2) 0.01193(18) 0.00610(18) 0.00637(18) Re4 0.0382(2) 0.0238(2) 0.0267(2) 0.01120(18) 0.00844(18) 0.00834(18) Re5 0.0408(3) 0.0263(2) 0.0251(2) 0.01094(18) 0.00686(18) 0.00428(18) Re6 0.0386(3) 0.0244(2) 0.0310(2) 0.01003(18) 0.01112(19) 0.00927(18) O1 0.027(4) 0.025(4) 0.039(4) 0.018(3) 0.001(3) -0.002(3) O2 0.038(4) 0.030(4) 0.036(4) 0.015(3) 0.013(3) 0.005(3) O3 0.055(5) 0.028(4) 0.022(4) 0.008(3) 0.007(3) 0.017(3) O4 0.034(4) 0.031(4) 0.040(4) 0.018(3) 0.010(3) 0.006(3) O5 0.043(4) 0.029(4) 0.042(4) 0.024(3) 0.015(3) 0.008(3) O6 0.044(4) 0.033(4) 0.033(4) 0.014(3) 0.011(3) 0.000(3) O7 0.038(4) 0.028(4) 0.037(4) 0.015(3) 0.015(3) 0.007(3) O8 0.062(5) 0.032(4) 0.034(4) 0.010(3) 0.016(4) 0.022(4) O9 0.040(4) 0.026(4) 0.026(4) 0.009(3) 0.008(3) 0.013(3) O10 0.059(5) 0.031(4) 0.028(4) 0.010(3) 0.006(3) 0.005(4) O11 0.060(5) 0.039(4) 0.020(4) 0.009(3) 0.007(3) 0.003(4) O12 0.041(4) 0.036(4) 0.036(4) 0.017(4) 0.010(3) 0.007(3) O13 0.048(5) 0.034(4) 0.034(4) 0.012(3) -0.002(3) -0.004(3) O14 0.058(5) 0.033(4) 0.038(4) 0.008(4) 0.018(4) 0.015(4) O15 0.056(5) 0.025(4) 0.036(4) 0.020(3) 0.012(3) 0.001(3) O16 0.054(5) 0.036(4) 0.035(4) 0.020(4) 0.010(4) -0.002(3) O17 0.040(4) 0.053(5) 0.048(5) 0.027(4) -0.003(4) 0.013(4) O18 0.052(5) 0.024(4) 0.036(4) 0.008(3) 0.005(3) -0.002(3) O19 0.042(5) 0.053(5) 0.060(5) 0.032(4) 0.014(4) 0.020(4) O20 0.062(5) 0.032(4) 0.044(5) 0.011(4) 0.016(4) 0.009(4) O21 0.067(5) 0.016(3) 0.041(4) 0.012(3) 0.015(4) 0.005(3) O22 0.054(5) 0.038(4) 0.039(4) 0.013(4) 0.001(4) 0.013(4) O23 0.038(4) 0.051(5) 0.052(5) 0.026(4) -0.003(4) 0.004(4) O24 0.067(5) 0.021(4) 0.046(5) 0.005(4) 0.015(4) 0.003(4) O25 0.046(5) 0.053(5) 0.031(4) 0.020(4) -0.001(3) 0.019(4) O26 0.055(5) 0.044(5) 0.060(5) 0.021(4) 0.012(4) 0.021(4) O27 0.062(5) 0.031(4) 0.036(4) 0.014(4) 0.011(4) 0.004(4) C1 0.037(6) 0.036(6) 0.043(7) 0.014(5) -0.001(5) -0.001(5) C2 0.036(6) 0.038(6) 0.048(7) 0.012(6) 0.007(5) -0.007(5) C3 0.044(7) 0.038(7) 0.073(9) 0.018(6) 0.022(6) -0.005(5) C4 0.050(7) 0.043(7) 0.060(8) 0.026(6) 0.023(6) 0.001(6) C5 0.036(7) 0.044(7) 0.077(9) 0.037(7) 0.010(6) 0.000(5) C6 0.066(8) 0.042(7) 0.047(8) 0.018(6) 0.005(6) 0.003(6) C7 0.054(8) 0.039(7) 0.052(8) 0.017(6) 0.007(6) -0.009(6) C8 0.066(8) 0.038(6) 0.026(6) 0.005(5) 0.004(5) -0.009(6) C9 0.077(9) 0.038(7) 0.058(8) 0.023(7) 0.012(7) -0.015(6) C10 0.069(9) 0.035(7) 0.035(7) -0.001(5) 0.005(6) 0.008(6) C11 0.063(8) 0.034(6) 0.034(6) 0.008(5) 0.004(6) 0.002(6) C12 0.086(10) 0.048(7) 0.041(7) 0.030(6) 0.007(6) -0.007(6) C13 0.092(10) 0.031(6) 0.063(9) 0.026(7) 0.015(8) -0.012(6) C14 0.079(9) 0.046(7) 0.031(7) 0.010(6) 0.009(6) 0.004(6) C15 0.082(9) 0.048(7) 0.044(7) 0.026(6) 0.011(7) -0.004(6) C16 0.064(8) 0.039(7) 0.041(7) 0.004(6) 0.018(6) 0.015(6) C17 0.092(10) 0.025(6) 0.053(8) 0.011(6) 0.033(7) 0.020(6) C18 0.121(13) 0.032(7) 0.074(10) 0.028(7) 0.027(9) -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 Re1 O25 1.682(7) . ? Re1 O21 1.886(6) . ? Re1 O1 1.891(6) . ? Re1 O20 1.936(7) . ? Re1 O7 2.074(6) . ? Re1 O12 2.140(6) 2_655 ? Re2 O23 1.675(7) . ? Re2 O1 1.876(6) . ? Re2 O27 1.892(6) . ? Re2 O13 1.901(7) . ? Re2 O12 2.062(6) . ? Re2 O7 2.180(6) 2_655 ? Re3 O17 1.669(7) . ? Re3 O9 1.881(6) . ? Re3 O15 1.907(6) . ? Re3 O10 1.923(6) . ? Re3 O4 2.074(6) . ? Re3 O5 2.148(6) . ? Re4 O19 1.674(7) . ? Re4 O18 1.894(6) . ? Re4 O3 1.901(6) . ? Re4 O8 1.911(6) . ? Re4 O5 2.062(6) . ? Re4 O4 2.179(6) . ? Re5 O22 1.674(7) . ? Re5 O3 1.886(6) . ? Re5 O16 1.893(6) . ? Re5 O11 1.917(6) . ? Re5 O6 2.069(6) . ? Re5 O2 2.155(6) . ? Re6 O26 1.665(8) . ? Re6 O24 1.883(7) . ? Re6 O9 1.905(5) . ? Re6 O14 1.919(6) . ? Re6 O2 2.046(6) . ? Re6 O6 2.189(7) . ? O2 C3 1.456(11) . ? O4 C1 1.445(10) . ? O5 C4 1.450(10) . ? O6 C2 1.474(10) . ? O7 C5 1.437(11) . ? O7 Re2 2.180(6) 2_655 ? O8 C17 1.425(10) . ? O10 C11 1.423(12) . ? O11 C8 1.403(11) . ? O12 C7 1.457(11) . ? O12 Re1 2.140(6) 2_655 ? O13 C14 1.400(11) . ? O14 C10 1.425(11) . ? O15 C15 1.420(11) . ? O16 C12 1.431(10) . ? O18 C9 1.440(11) . ? O20 C16 1.407(11) . ? O21 C18 1.440(11) . ? O24 C13 1.444(11) . ? O27 C6 1.457(11) . ? 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 O25 Re1 O21 107.7(3) . . ? O25 Re1 O1 95.1(3) . . ? O21 Re1 O1 88.4(3) . . ? O25 Re1 O20 95.6(3) . . ? O21 Re1 O20 86.7(3) . . ? O1 Re1 O20 169.2(3) . . ? O25 Re1 O7 92.0(3) . . ? O21 Re1 O7 160.0(3) . . ? O1 Re1 O7 93.2(2) . . ? O20 Re1 O7 88.2(3) . . ? O25 Re1 O12 162.4(3) . 2_655 ? O21 Re1 O12 89.8(3) . 2_655 ? O1 Re1 O12 84.0(2) . 2_655 ? O20 Re1 O12 86.3(3) . 2_655 ? O7 Re1 O12 70.6(2) . 2_655 ? O23 Re2 O1 93.9(3) . . ? O23 Re2 O27 104.7(3) . . ? O1 Re2 O27 94.8(3) . . ? O23 Re2 O13 99.3(3) . . ? O1 Re2 O13 166.2(3) . . ? O27 Re2 O13 85.8(3) . . ? O23 Re2 O12 95.1(3) . . ? O1 Re2 O12 90.1(2) . . ? O27 Re2 O12 159.2(3) . . ? O13 Re2 O12 84.6(3) . . ? O23 Re2 O7 164.5(3) . 2_655 ? O1 Re2 O7 82.1(2) . 2_655 ? O27 Re2 O7 90.6(3) . 2_655 ? O13 Re2 O7 84.2(3) . 2_655 ? O12 Re2 O7 70.0(2) . 2_655 ? O17 Re3 O9 94.7(3) . . ? O17 Re3 O15 107.5(3) . . ? O9 Re3 O15 89.0(3) . . ? O17 Re3 O10 97.3(3) . . ? O9 Re3 O10 168.0(3) . . ? O15 Re3 O10 86.1(3) . . ? O17 Re3 O4 92.7(3) . . ? O9 Re3 O4 93.1(2) . . ? O15 Re3 O4 159.5(3) . . ? O10 Re3 O4 87.7(2) . . ? O17 Re3 O5 162.9(3) . . ? O9 Re3 O5 83.3(2) . . ? O15 Re3 O5 89.5(3) . . ? O10 Re3 O5 85.7(3) . . ? O4 Re3 O5 70.5(2) . . ? O19 Re4 O18 105.2(3) . . ? O19 Re4 O3 94.9(3) . . ? O18 Re4 O3 93.4(3) . . ? O19 Re4 O8 97.6(3) . . ? O18 Re4 O8 85.7(3) . . ? O3 Re4 O8 167.2(3) . . ? O19 Re4 O5 95.0(3) . . ? O18 Re4 O5 158.2(3) . . ? O3 Re4 O5 93.0(2) . . ? O8 Re4 O5 83.5(3) . . ? O19 Re4 O4 164.6(3) . . ? O18 Re4 O4 90.2(3) . . ? O3 Re4 O4 82.0(3) . . ? O8 Re4 O4 85.2(3) . . ? O5 Re4 O4 70.1(2) . . ? O22 Re5 O3 95.0(3) . . ? O22 Re5 O16 107.1(3) . . ? O3 Re5 O16 88.6(3) . . ? O22 Re5 O11 97.1(3) . . ? O3 Re5 O11 167.7(3) . . ? O16 Re5 O11 85.8(3) . . ? O22 Re5 O6 92.8(3) . . ? O3 Re5 O6 93.3(2) . . ? O16 Re5 O6 159.8(3) . . ? O11 Re5 O6 88.3(3) . . ? O22 Re5 O2 162.8(3) . . ? O3 Re5 O2 83.6(3) . . ? O16 Re5 O2 90.0(3) . . ? O11 Re5 O2 85.5(3) . . ? O6 Re5 O2 70.3(2) . . ? O26 Re6 O24 105.7(3) . . ? O26 Re6 O9 95.1(3) . . ? O24 Re6 O9 93.6(3) . . ? O26 Re6 O14 98.6(3) . . ? O24 Re6 O14 86.1(3) . . ? O9 Re6 O14 165.9(3) . . ? O26 Re6 O2 95.1(3) . . ? O24 Re6 O2 158.2(3) . . ? O9 Re6 O2 91.1(2) . . ? O14 Re6 O2 84.1(3) . . ? O26 Re6 O6 164.6(3) . . ? O24 Re6 O6 89.6(3) . . ? O9 Re6 O6 81.9(2) . . ? O14 Re6 O6 84.0(3) . . ? O2 Re6 O6 70.0(2) . . ? Re2 O1 Re1 161.0(3) . . ? C3 O2 Re6 119.0(5) . . ? C3 O2 Re5 121.0(6) . . ? Re6 O2 Re5 110.8(3) . . ? Re5 O3 Re4 161.9(4) . . ? C1 O4 Re3 120.6(5) . . ? C1 O4 Re4 121.5(5) . . ? Re3 O4 Re4 108.7(3) . . ? C4 O5 Re4 119.1(5) . . ? C4 O5 Re3 121.6(6) . . ? Re4 O5 Re3 110.3(3) . . ? C2 O6 Re5 119.0(5) . . ? C2 O6 Re6 120.5(5) . . ? Re5 O6 Re6 108.6(3) . . ? C5 O7 Re1 119.6(6) . . ? C5 O7 Re2 120.5(5) . 2_655 ? Re1 O7 Re2 108.5(3) . 2_655 ? C17 O8 Re4 129.1(6) . . ? Re3 O9 Re6 157.5(4) . . ? C11 O10 Re3 124.4(6) . . ? C8 O11 Re5 128.4(6) . . ? C7 O12 Re2 119.1(6) . . ? C7 O12 Re1 120.5(5) . 2_655 ? Re2 O12 Re1 110.5(3) . 2_655 ? C14 O13 Re2 129.0(6) . . ? C10 O14 Re6 129.8(6) . . ? C15 O15 Re3 128.6(6) . . ? C12 O16 Re5 129.2(6) . . ? C9 O18 Re4 128.9(6) . . ? C16 O20 Re1 127.0(7) . . ? C18 O21 Re1 129.8(6) . . ? C13 O24 Re6 127.7(6) . . ? C6 O27 Re2 126.7(6) . . ? _diffrn_measured_fraction_theta_max 0.861 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.861 _refine_diff_density_max 2.176 _refine_diff_density_min -1.626 _refine_diff_density_rms 0.232 #========================================================================== #==================================================================== #Compound 3a data_remos _database_code_CSD 152227 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H36 Mo1.0 O18 Re3.0' _chemical_formula_weight 1122.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Re' 'Re' -1.0185 7.2310 '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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 7.9141(4) _cell_length_b 16.0535(8) _cell_length_c 17.5938(9) _cell_angle_alpha 113.322(1) _cell_angle_beta 93.355(1) _cell_angle_gamma 92.754(1) _cell_volume 2042.95(30) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 999(I>10sigma(I)) _cell_measurement_theta_min 1.40 _cell_measurement_theta_max 22.50 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.739 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 519 _exptl_absorpt_coefficient_mu 4.606 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.1199 _exptl_absorpt_correction_T_max 0.3922 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K' _diffrn_measurement_method SMART CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8913 _diffrn_reflns_av_R_equivalents 0.0551 _diffrn_reflns_av_sigmaI/netI 0.1075 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 22.50 _reflns_number_total 5302 _reflns_number_gt 3305 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.1035P)^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 0.00021(7) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5302 _refine_ls_number_parameters 467 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0953 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1632 _refine_ls_wR_factor_gt 0.1575 _refine_ls_goodness_of_fit_ref 0.897 _refine_ls_restrained_S_all 0.897 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 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 Re1 Re 0.41861(15) 0.15937(8) 0.04836(8) 0.0406(5) Uani 0.708(5) 1 d P . . Mo1 Mo 0.41861(15) 0.15937(8) 0.04836(8) 0.0406(5) Uani 0.29 1 d P . . Re2 Re 0.36647(13) -0.04528(7) -0.14875(7) 0.0388(5) Uani 0.828(5) 1 d P . . Mo2 Mo 0.36647(13) -0.04528(7) -0.14875(7) 0.0388(5) Uani 0.17 1 d P . . Re3 Re 0.20044(14) 0.31171(7) 0.79420(7) 0.0358(5) Uani 0.693(5) 1 d P . . Mo3 Mo 0.20044(14) 0.31171(7) 0.79420(7) 0.0358(5) Uani 0.31 1 d P . . Re4 Re -0.00796(13) 0.46278(7) 0.73393(7) 0.0368(5) Uani 0.804(5) 1 d P . . Mo4 Mo -0.00796(13) 0.46278(7) 0.73393(7) 0.0368(5) Uani 0.20 1 d P . . Re5 Re 0.10213(15) 0.33109(8) 0.51844(7) 0.0365(5) Uani 0.615(5) 1 d P . . Mo5 Mo 0.10213(15) 0.33109(8) 0.51844(7) 0.0365(5) Uani 0.39 1 d P . . Re6 Re 0.30402(13) 0.17858(7) 0.57963(7) 0.0404(5) Uani 0.873(5) 1 d P . . Mo6 Mo 0.30402(13) 0.17858(7) 0.57963(7) 0.0404(5) Uani 0.13 1 d P . . O1 O 0.073(2) 0.3976(11) 0.6301(13) 0.070(7) Uani 1 1 d . . . O2 O 0.419(2) 0.0528(10) -0.0498(12) 0.065(6) Uani 1 1 d . . . O3 O 0.068(2) 0.2084(10) 0.5309(11) 0.054(5) Uani 1 1 d . . . O4 O 0.212(2) 0.2410(12) 0.6768(11) 0.055(5) Uani 1 1 d . . . O5 O 0.215(2) 0.4329(12) 0.5102(12) 0.068(6) Uani 1 1 d . . . O6 O 0.134(2) 0.3854(13) 0.9093(12) 0.075(6) Uani 1 1 d . . . O7 O 0.661(2) 0.1265(10) 0.0853(10) 0.050(5) Uani 1 1 d . . . O8 O 0.210(2) 0.0662(13) 0.5683(11) 0.066(6) Uani 1 1 d . . . O9 O 0.467(2) 0.0070(14) -0.2172(11) 0.069(6) Uani 1 1 d . . . O10 O 0.505(2) 0.1839(12) 0.6200(15) 0.042(6) Uani 0.70 1 d P . . O11 O 0.087(2) 0.5751(12) 0.7465(12) 0.069(6) Uani 1 1 d . . . O12 O -0.209(2) 0.4562(12) 0.6957(14) 0.074(6) Uani 1 1 d . . . O13 O 0.2331(19) 0.4326(10) 0.7788(11) 0.050(5) Uani 1 1 d . . . O14 O 0.348(2) 0.1212(14) 0.4636(13) 0.073(6) Uani 1 1 d . . . O15 O 0.524(2) 0.2279(12) -0.0032(11) 0.066(5) Uani 1 1 d . . . O16 O 0.385(2) 0.0840(11) 0.1188(11) 0.058(5) Uani 1 1 d . . . O17 O 0.182(2) 0.2605(15) 0.4045(13) 0.082(7) Uani 1 1 d . . . O18 O 0.210(2) 0.1680(12) 0.0398(11) 0.061(5) Uani 1 1 d . . . O19 O 0.161(2) -0.0256(13) -0.1503(10) 0.058(5) Uani 1 1 d . . . O20 O 0.351(2) -0.1586(12) -0.2444(13) 0.069(6) Uani 1 1 d . . . O21 O -0.0401(19) 0.3462(10) 0.7550(10) 0.049(5) Uani 1 1 d . . . O22 O 0.089(2) 0.2101(12) 0.8067(12) 0.062(5) Uani 1 1 d . . . O23 O -0.103(2) 0.3279(13) 0.4853(14) 0.085(7) Uani 1 1 d . . . O24 O 0.457(3) 0.2679(13) 0.1503(14) 0.088(7) Uani 1 1 d . . . O25 O -0.047(3) 0.5236(13) 0.8511(12) 0.073(6) Uani 1 1 d . . . O26 O 0.3415(19) 0.2975(10) 0.5611(11) 0.049(5) Uani 1 1 d . . . O27 O 0.412(2) 0.3124(12) 0.8168(13) 0.068(6) Uani 1 1 d . . . C1 C 0.233(3) 0.0284(17) 0.111(2) 0.069(9) Uani 1 1 d . . . H1A H 0.2435 -0.0001 0.1498 0.104 Uiso 1 1 calc R . . H1B H 0.2151 -0.0175 0.0558 0.104 Uiso 1 1 calc R . . H1C H 0.1380 0.0654 0.1230 0.104 Uiso 1 1 calc R . . C2 C 0.128(4) 0.0428(19) 0.6318(19) 0.071(9) Uani 1 1 d . . . H2A H 0.0903 -0.0208 0.6086 0.107 Uiso 1 1 calc R . . H2B H 0.0314 0.0782 0.6489 0.107 Uiso 1 1 calc R . . H2C H 0.2076 0.0558 0.6788 0.107 Uiso 1 1 calc R . . C3 C 0.170(3) 0.5980(19) 0.6797(18) 0.063(8) Uani 1 1 d . . . H3A H 0.2078 0.6615 0.7020 0.095 Uiso 1 1 calc R . . H3B H 0.0893 0.5843 0.6329 0.095 Uiso 1 1 calc R . . H3C H 0.2662 0.5624 0.6625 0.095 Uiso 1 1 calc R . . C4 C 0.515(4) 0.1020(16) -0.196(2) 0.088(11) Uani 1 1 d . . . H4A H 0.5640 0.1091 -0.2415 0.132 Uiso 1 1 calc R . . H4B H 0.5968 0.1242 -0.1482 0.132 Uiso 1 1 calc R . . H4C H 0.4162 0.1360 -0.1827 0.132 Uiso 1 1 calc R . . C5 C 0.388(3) 0.4619(18) 0.7579(19) 0.065(8) Uani 1 1 d . . . H5A H 0.4811 0.4426 0.7828 0.098 Uiso 1 1 calc R . . H5B H 0.3974 0.5271 0.7780 0.098 Uiso 1 1 calc R . . H5C H 0.3915 0.4361 0.6987 0.098 Uiso 1 1 calc R . . C6 C 0.808(3) 0.1901(18) 0.106(2) 0.079(10) Uani 1 1 d . . . H6A H 0.9046 0.1639 0.1208 0.118 Uiso 1 1 calc R . . H6B H 0.7878 0.2451 0.1515 0.118 Uiso 1 1 calc R . . H6C H 0.8305 0.2035 0.0586 0.118 Uiso 1 1 calc R . . C7 C 0.260(4) 0.447(2) 0.439(2) 0.081(10) Uani 1 1 d . . . H7A H 0.3153 0.5075 0.4558 0.121 Uiso 1 1 calc R . . H7B H 0.1599 0.4414 0.4031 0.121 Uiso 1 1 calc R . . H7C H 0.3367 0.4032 0.4093 0.121 Uiso 1 1 calc R . . C8 C -0.096(3) 0.1822(17) 0.5517(16) 0.052(7) Uani 1 1 d . . . H8A H -0.1855 0.2011 0.5242 0.078 Uiso 1 1 calc R . . H8B H -0.1030 0.2108 0.6106 0.078 Uiso 1 1 calc R . . H8C H -0.1091 0.1173 0.5341 0.078 Uiso 1 1 calc R . . C9 C -0.077(5) 0.615(2) 0.893(2) 0.093(12) Uani 1 1 d . . . H9A H -0.0914 0.6270 0.9503 0.139 Uiso 1 1 calc R . . H9B H -0.1776 0.6279 0.8683 0.139 Uiso 1 1 calc R . . H9C H 0.0184 0.6528 0.8903 0.139 Uiso 1 1 calc R . . C10 C 0.373(5) 0.031(2) 0.4156(19) 0.091(11) Uani 1 1 d . . . H10A H 0.3931 0.0242 0.3603 0.136 Uiso 1 1 calc R . . H10B H 0.2744 -0.0073 0.4139 0.136 Uiso 1 1 calc R . . H10C H 0.4702 0.0130 0.4395 0.136 Uiso 1 1 calc R . . C11 C -0.200(3) 0.3251(19) 0.7853(19) 0.061(8) Uani 1 1 d . . . H11A H -0.2935 0.3449 0.7611 0.092 Uiso 1 1 calc R . . H11B H -0.1943 0.3560 0.8446 0.092 Uiso 1 1 calc R . . H11C H -0.2167 0.2606 0.7699 0.092 Uiso 1 1 calc R . . C12 C 0.360(4) 0.291(3) 0.222(2) 0.107(14) Uani 1 1 d . . . H12A H 0.4054 0.3488 0.2634 0.161 Uiso 1 1 calc R . . H12B H 0.3653 0.2452 0.2432 0.161 Uiso 1 1 calc R . . H12C H 0.2434 0.2959 0.2056 0.161 Uiso 1 1 calc R . . C13 C 0.228(3) 0.4673(16) 0.9642(16) 0.057(7) Uani 1 1 d . . . H13A H 0.1757 0.4919 1.0154 0.085 Uiso 1 1 calc R . . H13B H 0.2306 0.5107 0.9391 0.085 Uiso 1 1 calc R . . H13C H 0.3425 0.4543 0.9748 0.085 Uiso 1 1 calc R . . C14 C 0.094(4) 0.179(2) 0.3451(18) 0.089(11) Uani 1 1 d . . . H14A H 0.1534 0.1574 0.2958 0.134 Uiso 1 1 calc R . . H14B H -0.0189 0.1921 0.3318 0.134 Uiso 1 1 calc R . . H14C H 0.0872 0.1340 0.3678 0.134 Uiso 1 1 calc R . . C15 C 0.499(3) 0.3155(18) 0.5354(18) 0.069(10) Uani 1 1 d . . . H15A H 0.5881 0.2952 0.5619 0.103 Uiso 1 1 calc R . . H15B H 0.5193 0.3798 0.5504 0.103 Uiso 1 1 calc R . . H15C H 0.4987 0.2840 0.4763 0.103 Uiso 1 1 calc R . . C16 C 0.050(5) 0.201(2) 0.880(2) 0.088(11) Uani 1 1 d . . . H16A H -0.0063 0.1420 0.8664 0.132 Uiso 1 1 calc R . . H16B H -0.0244 0.2470 0.9089 0.132 Uiso 1 1 calc R . . H16C H 0.1522 0.2083 0.9146 0.132 Uiso 1 1 calc R . . C17 C 0.391(4) -0.167(3) -0.3263(17) 0.094(13) Uani 1 1 d . . . H17A H 0.3735 -0.2295 -0.3645 0.140 Uiso 1 1 calc R . . H17B H 0.5083 -0.1460 -0.3241 0.140 Uiso 1 1 calc R . . H17C H 0.3195 -0.1308 -0.3446 0.140 Uiso 1 1 calc R . . C18 C 0.563(4) 0.3238(15) 0.0219(18) 0.069(9) Uani 1 1 d . . . H18A H 0.6193 0.3344 -0.0207 0.103 Uiso 1 1 calc R . . H18B H 0.6359 0.3472 0.0724 0.103 Uiso 1 1 calc R . . H18C H 0.4595 0.3541 0.0308 0.103 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 Re1 0.0447(8) 0.0353(7) 0.0394(9) 0.0106(6) 0.0104(5) 0.0121(5) Mo1 0.0447(8) 0.0353(7) 0.0394(9) 0.0106(6) 0.0104(5) 0.0121(5) Re2 0.0390(7) 0.0373(7) 0.0358(8) 0.0095(5) 0.0055(5) 0.0068(4) Mo2 0.0390(7) 0.0373(7) 0.0358(8) 0.0095(5) 0.0055(5) 0.0068(4) Re3 0.0402(8) 0.0335(7) 0.0333(9) 0.0110(6) 0.0094(5) 0.0121(5) Mo3 0.0402(8) 0.0335(7) 0.0333(9) 0.0110(6) 0.0094(5) 0.0121(5) Re4 0.0404(7) 0.0329(7) 0.0364(8) 0.0112(5) 0.0092(5) 0.0122(5) Mo4 0.0404(7) 0.0329(7) 0.0364(8) 0.0112(5) 0.0092(5) 0.0122(5) Re5 0.0419(8) 0.0348(8) 0.0308(9) 0.0095(6) 0.0091(5) 0.0093(5) Mo5 0.0419(8) 0.0348(8) 0.0308(9) 0.0095(6) 0.0091(5) 0.0093(5) Re6 0.0410(7) 0.0362(7) 0.0417(9) 0.0106(5) 0.0136(5) 0.0150(5) Mo6 0.0410(7) 0.0362(7) 0.0417(9) 0.0106(5) 0.0136(5) 0.0150(5) O1 0.064(12) 0.055(12) 0.121(18) 0.051(12) 0.093(12) 0.030(9) O2 0.070(13) 0.028(9) 0.087(16) 0.022(9) -0.035(10) -0.022(8) O3 0.045(11) 0.036(10) 0.070(14) 0.008(9) 0.010(9) 0.014(8) O4 0.047(11) 0.072(13) 0.061(13) 0.035(10) 0.048(9) 0.019(9) O5 0.071(14) 0.058(12) 0.065(15) 0.012(11) 0.002(10) 0.010(10) O6 0.077(14) 0.073(14) 0.060(14) 0.008(11) 0.047(10) -0.014(10) O7 0.056(11) 0.039(10) 0.044(12) 0.006(8) 0.001(8) 0.011(8) O8 0.054(12) 0.076(13) 0.055(14) 0.005(11) 0.022(9) 0.047(10) O9 0.082(14) 0.107(17) 0.027(12) 0.033(11) 0.011(9) 0.016(12) O10 0.004(10) 0.020(11) 0.098(19) 0.020(11) -0.017(10) 0.003(8) O11 0.050(12) 0.066(13) 0.071(15) 0.000(11) 0.015(10) 0.033(9) O12 0.045(12) 0.057(12) 0.126(19) 0.044(12) 0.000(11) 0.013(9) O13 0.032(9) 0.041(10) 0.067(13) 0.009(9) 0.006(8) 0.014(7) O14 0.069(13) 0.081(15) 0.085(16) 0.041(13) 0.058(11) 0.029(11) O15 0.089(15) 0.059(13) 0.057(14) 0.028(10) 0.017(10) 0.017(10) O16 0.037(10) 0.040(10) 0.083(15) 0.010(9) 0.003(9) 0.016(8) O17 0.072(14) 0.095(17) 0.071(16) 0.021(13) 0.045(11) 0.001(11) O18 0.056(12) 0.065(12) 0.073(14) 0.031(11) 0.048(10) 0.027(9) O19 0.055(12) 0.091(14) 0.041(12) 0.038(10) 0.018(8) 0.021(10) O20 0.062(13) 0.053(12) 0.086(17) 0.028(11) -0.023(10) -0.019(9) O21 0.042(10) 0.039(10) 0.061(13) 0.012(9) 0.011(8) 0.017(7) O22 0.056(12) 0.052(11) 0.061(15) 0.005(10) 0.004(9) 0.014(9) O23 0.042(12) 0.079(14) 0.13(2) 0.038(13) -0.015(11) 0.017(10) O24 0.114(18) 0.052(13) 0.088(18) 0.022(12) -0.001(13) -0.030(12) O25 0.091(15) 0.068(13) 0.075(15) 0.035(12) 0.055(12) 0.034(11) O26 0.037(10) 0.038(9) 0.066(13) 0.016(9) -0.002(8) 0.006(7) O27 0.049(12) 0.052(11) 0.114(18) 0.044(11) 0.000(10) 0.004(9) C1 0.046(18) 0.044(17) 0.11(3) 0.031(17) -0.002(16) -0.005(13) C2 0.07(2) 0.054(19) 0.09(3) 0.018(17) 0.037(17) 0.000(14) C3 0.065(19) 0.060(19) 0.07(2) 0.026(17) 0.047(16) 0.015(14) C4 0.11(3) 0.011(14) 0.15(3) 0.042(17) 0.01(2) -0.014(14) C5 0.049(18) 0.054(18) 0.09(2) 0.027(16) -0.001(15) -0.006(13) C6 0.06(2) 0.046(18) 0.12(3) 0.025(18) 0.013(17) -0.022(14) C7 0.09(3) 0.09(3) 0.08(3) 0.05(2) 0.015(19) 0.003(19) C8 0.041(16) 0.055(17) 0.054(19) 0.016(14) 0.008(12) -0.008(12) C9 0.15(3) 0.06(2) 0.07(3) 0.020(18) 0.07(2) 0.07(2) C10 0.13(3) 0.07(2) 0.05(2) -0.006(18) 0.05(2) 0.03(2) C11 0.034(15) 0.07(2) 0.09(2) 0.044(17) 0.014(14) 0.004(13) C12 0.11(3) 0.13(3) 0.05(2) 0.00(2) 0.07(2) 0.03(2) C13 0.071(19) 0.036(15) 0.044(19) -0.001(13) 0.003(13) -0.009(13) C14 0.12(3) 0.07(2) 0.04(2) -0.015(17) 0.015(18) 0.01(2) C15 0.023(14) 0.057(18) 0.10(2) 0.002(16) 0.022(14) -0.025(11) C16 0.13(3) 0.07(2) 0.08(3) 0.05(2) -0.01(2) -0.03(2) C17 0.08(2) 0.19(4) 0.032(19) 0.06(2) 0.054(16) 0.05(2) C18 0.10(2) 0.022(15) 0.08(2) 0.013(15) 0.042(17) -0.016(13) _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 Re1 O18 1.664(17) . ? Re1 O15 1.876(19) . ? Re1 O2 1.891(17) . ? Re1 O24 1.94(2) . ? Re1 O16 2.067(19) . ? Re1 O7 2.142(16) . ? Re2 O19 1.668(16) . ? Re2 O2 1.837(16) . ? Re2 O9 1.907(19) . ? Re2 O20 1.922(18) . ? Re2 O7 2.035(17) 2_655 ? Re2 O16 2.189(16) 2_655 ? Re3 O27 1.691(17) . ? Re3 O22 1.91(2) . ? Re3 O4 1.936(17) . ? Re3 O6 2.019(18) . ? Re3 O13 2.070(17) . ? Re3 O21 2.156(15) . ? Re4 O12 1.674(17) . ? Re4 O11 1.84(2) . ? Re4 O1 1.881(16) . ? Re4 O25 1.953(19) . ? Re4 O21 2.054(17) . ? Re4 O13 2.169(15) . ? Re5 O23 1.683(18) . ? Re5 O1 1.863(19) . ? Re5 O5 1.88(2) . ? Re5 O17 2.032(19) . ? Re5 O3 2.071(17) . ? Re5 O26 2.165(15) . ? Re6 O10 1.687(17) . ? Re6 O4 1.822(15) . ? Re6 O8 1.85(2) . ? Re6 O14 1.940(19) . ? Re6 O26 2.069(16) . ? Re6 O3 2.161(16) . ? O3 C8 1.46(3) . ? O5 C7 1.43(3) . ? O6 C13 1.43(3) . ? O7 C6 1.44(3) . ? O7 Mo2 2.035(17) 2_655 ? O7 Re2 2.035(17) 2_655 ? O8 C2 1.48(3) . ? O9 C4 1.44(3) . ? O11 C3 1.54(3) . ? O13 C5 1.41(3) . ? O14 C10 1.39(3) . ? O15 C18 1.44(3) . ? O16 C1 1.43(3) . ? O16 Mo2 2.189(16) 2_655 ? O16 Re2 2.189(16) 2_655 ? O17 C14 1.43(3) . ? O20 C17 1.45(3) . ? O21 C11 1.48(3) . ? O22 C16 1.40(3) . ? O24 C12 1.44(3) . ? O25 C9 1.40(3) . ? O26 C15 1.41(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 O18 Re1 O15 108.1(8) . . ? O18 Re1 O2 95.3(8) . . ? O15 Re1 O2 90.3(8) . . ? O18 Re1 O24 93.9(9) . . ? O15 Re1 O24 86.4(9) . . ? O2 Re1 O24 170.8(9) . . ? O18 Re1 O16 90.5(7) . . ? O15 Re1 O16 161.0(7) . . ? O2 Re1 O16 91.7(7) . . ? O24 Re1 O16 88.7(8) . . ? O18 Re1 O7 160.9(8) . . ? O15 Re1 O7 90.8(7) . . ? O2 Re1 O7 87.0(6) . . ? O24 Re1 O7 84.4(8) . . ? O16 Re1 O7 70.4(6) . . ? O19 Re2 O2 92.8(8) . . ? O19 Re2 O9 106.2(8) . . ? O2 Re2 O9 96.7(8) . . ? O19 Re2 O20 97.8(8) . . ? O2 Re2 O20 167.8(7) . . ? O9 Re2 O20 86.2(8) . . ? O19 Re2 O7 94.1(7) . 2_655 ? O2 Re2 O7 89.3(7) . 2_655 ? O9 Re2 O7 158.5(7) . 2_655 ? O20 Re2 O7 84.0(7) . 2_655 ? O19 Re2 O16 163.5(8) . 2_655 ? O2 Re2 O16 82.6(7) . 2_655 ? O9 Re2 O16 90.1(8) . 2_655 ? O20 Re2 O16 85.6(7) . 2_655 ? O7 Re2 O16 70.1(7) 2_655 2_655 ? O27 Re3 O22 108.2(8) . . ? O27 Re3 O4 93.7(9) . . ? O22 Re3 O4 91.0(7) . . ? O27 Re3 O6 99.0(9) . . ? O22 Re3 O6 85.5(8) . . ? O4 Re3 O6 167.3(8) . . ? O27 Re3 O13 91.6(7) . . ? O22 Re3 O13 159.9(7) . . ? O4 Re3 O13 91.6(7) . . ? O6 Re3 O13 87.6(7) . . ? O27 Re3 O21 161.5(8) . . ? O22 Re3 O21 90.3(7) . . ? O4 Re3 O21 83.9(7) . . ? O6 Re3 O21 84.0(8) . . ? O13 Re3 O21 70.2(6) . . ? O12 Re4 O11 106.0(8) . . ? O12 Re4 O1 94.6(10) . . ? O11 Re4 O1 96.0(8) . . ? O12 Re4 O25 97.3(9) . . ? O11 Re4 O25 84.6(8) . . ? O1 Re4 O25 167.5(9) . . ? O12 Re4 O21 94.2(8) . . ? O11 Re4 O21 157.8(8) . . ? O1 Re4 O21 91.2(7) . . ? O25 Re4 O21 84.0(7) . . ? O12 Re4 O13 164.0(8) . . ? O11 Re4 O13 89.9(7) . . ? O1 Re4 O13 82.4(8) . . ? O25 Re4 O13 85.1(7) . . ? O21 Re4 O13 70.2(6) . . ? O23 Re5 O1 95.3(10) . . ? O23 Re5 O5 106.9(9) . . ? O1 Re5 O5 91.4(8) . . ? O23 Re5 O17 95.9(10) . . ? O1 Re5 O17 168.8(9) . . ? O5 Re5 O17 84.9(8) . . ? O23 Re5 O3 93.0(8) . . ? O1 Re5 O3 92.2(7) . . ? O5 Re5 O3 159.3(7) . . ? O17 Re5 O3 87.8(8) . . ? O23 Re5 O26 163.4(8) . . ? O1 Re5 O26 86.2(7) . . ? O5 Re5 O26 89.6(7) . . ? O17 Re5 O26 83.2(8) . . ? O3 Re5 O26 70.3(6) . . ? O10 Re6 O4 97.3(10) . . ? O10 Re6 O8 104.4(8) . . ? O4 Re6 O8 94.6(7) . . ? O10 Re6 O14 97.3(10) . . ? O4 Re6 O14 164.5(8) . . ? O8 Re6 O14 86.9(8) . . ? O10 Re6 O26 94.2(8) . . ? O4 Re6 O26 90.2(7) . . ? O8 Re6 O26 160.0(7) . . ? O14 Re6 O26 83.4(7) . . ? O10 Re6 O3 164.4(8) . . ? O4 Re6 O3 80.7(7) . . ? O8 Re6 O3 91.2(7) . . ? O14 Re6 O3 83.8(7) . . ? O26 Re6 O3 70.4(6) . . ? Re5 O1 Re4 167.0(12) . . ? Re2 O2 Re1 166.2(10) . . ? C8 O3 Re5 119.2(14) . . ? C8 O3 Re6 121.8(16) . . ? Re5 O3 Re6 109.6(7) . . ? Re6 O4 Re3 159.1(10) . . ? C7 O5 Re5 130.2(18) . . ? C13 O6 Re3 122.4(15) . . ? C6 O7 Mo2 119.2(17) . 2_655 ? C6 O7 Re2 119.2(17) . 2_655 ? Mo2 O7 Re2 0.00(7) 2_655 2_655 ? C6 O7 Re1 121.0(16) . . ? Mo2 O7 Re1 111.2(8) 2_655 . ? Re2 O7 Re1 111.2(8) 2_655 . ? C2 O8 Re6 127.7(16) . . ? C4 O9 Re2 127.0(18) . . ? C3 O11 Re4 126.2(15) . . ? C5 O13 Re3 122.4(15) . . ? C5 O13 Re4 120.8(17) . . ? Re3 O13 Re4 109.2(7) . . ? C10 O14 Re6 129.7(19) . . ? C18 O15 Re1 132.6(16) . . ? C1 O16 Re1 123.1(16) . . ? C1 O16 Mo2 121.3(15) . 2_655 ? Re1 O16 Mo2 108.2(8) . 2_655 ? C1 O16 Re2 121.3(15) . 2_655 ? Re1 O16 Re2 108.2(8) . 2_655 ? Mo2 O16 Re2 0.00(7) 2_655 2_655 ? C14 O17 Re5 123.3(18) . . ? C17 O20 Re2 124(2) . . ? C11 O21 Re4 120.0(14) . . ? C11 O21 Re3 121.2(15) . . ? Re4 O21 Re3 110.3(7) . . ? C16 O22 Re3 128.7(17) . . ? C12 O24 Re1 126(2) . . ? C9 O25 Re4 126.6(19) . . ? C15 O26 Re6 117.9(16) . . ? C15 O26 Re5 123.5(18) . . ? Re6 O26 Re5 109.5(7) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.765 _refine_diff_density_min -2.987 _refine_diff_density_rms 0.371 #========================================================================== #==================================================================== #Compound 3b data_moreme11 _database_code_CSD 152228 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H36 Mo2.4 O18 Re1.6' _chemical_formula_weight 996.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Re' 'Re' -1.0185 7.2310 '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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _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 7.905(2) _cell_length_b 15.997(4) _cell_length_c 17.519(6) _cell_angle_alpha 113.41(2) _cell_angle_beta 92.92(2) _cell_angle_gamma 92.71(3) _cell_volume 2024.9(10) _cell_formula_units_Z 3 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6485 _cell_measurement_theta_min 1.39 _cell_measurement_theta_max 28.00 _exptl_crystal_description prism _exptl_crystal_colour reddish black _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 473 _exptl_absorpt_coefficient_mu 2.771 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.3110 _exptl_absorpt_correction_T_max 0.4903 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART CCD 1K' _diffrn_measurement_method SMART CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11977 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.1169 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 28.40 _reflns_number_total 8733 _reflns_number_gt 5036 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0565P)^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 0.00060(6) _refine_ls_extinction_expression 'Fc^*^==kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8733 _refine_ls_number_parameters 485 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0745 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1242 _refine_ls_wR_factor_gt 0.1214 _refine_ls_goodness_of_fit_ref 0.816 _refine_ls_restrained_S_all 0.846 _refine_ls_shift/su_max 0.191 _refine_ls_shift/su_mean 0.005 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 Re1 Re -0.42000(9) 0.83909(5) 0.95060(5) 0.0351(3) Uani 0.521(4) 1 d P . . Mo1 Mo -0.42000(9) 0.83909(5) 0.95060(5) 0.0351(3) Uani 0.48 1 d P . . Re2 Re -0.36352(8) 1.04507(5) 1.14761(5) 0.0354(3) Uani 0.543(4) 1 d P . . Mo2 Mo -0.36352(8) 1.04507(5) 1.14761(5) 0.0354(3) Uani 0.46 1 d P . . Re3 Re -0.19840(8) 0.68765(4) 1.20487(5) 0.0317(3) Uani 0.494(4) 1 d P . . Mo3 Mo -0.19840(8) 0.68765(4) 1.20487(5) 0.0317(3) Uani 0.51 1 d P . . Re4 Re 0.00989(8) 0.53776(4) 1.26640(4) 0.0315(2) Uani 0.497(4) 1 d P . . Mo4 Mo 0.00989(8) 0.53776(4) 1.26640(4) 0.0315(2) Uani 0.50 1 d P . . Re5 Re -0.10130(9) 0.66924(5) 1.48279(5) 0.0326(3) Uani 0.473(4) 1 d P . . Mo5 Mo -0.10130(9) 0.66924(5) 1.48279(5) 0.0326(3) Uani 0.53 1 d P . . Re6 Re -0.30321(8) 0.82040(4) 1.42017(5) 0.0347(3) Uani 0.512(4) 1 d P . . Mo6 Mo -0.30321(8) 0.82040(4) 1.42017(5) 0.0347(3) Uani 0.49 1 d P . . O1 O -0.0796(13) 0.6015(6) 1.3689(8) 0.072(3) Uani 1 1 d . . . O2 O -0.4283(13) 0.9439(9) 1.0471(8) 0.083(4) Uani 1 1 d . . . O3 O -0.0639(12) 0.7912(7) 1.4712(7) 0.059(3) Uani 1 1 d . . . O4 O -0.2103(13) 0.7557(7) 1.3195(8) 0.069(3) Uani 1 1 d . . . O5 O -0.2131(14) 0.5634(7) 1.4870(7) 0.071(3) Uani 1 1 d . . . O6 O -0.1408(14) 0.6191(8) 1.0949(8) 0.077(3) Uani 1 1 d . . . O7 O -0.6644(13) 0.8733(7) 0.9161(8) 0.074(4) Uani 1 1 d . . . O8 O -0.2082(15) 0.9333(8) 1.4326(8) 0.081(4) Uani 1 1 d . . . O9 O -0.4614(15) 0.9938(9) 1.2158(8) 0.087(4) Uani 1 1 d . . . O10 O -0.4980(14) 0.8123(8) 1.3723(9) 0.049(4) Uani 0.70 1 d P . . O11 O -0.0838(15) 0.4242(8) 1.2574(7) 0.072(3) Uani 1 1 d . . . O12 O 0.2082(14) 0.5468(9) 1.3113(9) 0.092(4) Uani 1 1 d . . . O13 O -0.2318(13) 0.5652(7) 1.2166(7) 0.063(3) Uani 1 1 d . . . O14 O -0.3512(14) 0.8797(7) 1.5326(7) 0.075(3) Uani 1 1 d . . . O15 O -0.5256(15) 0.7726(8) 1.0055(8) 0.081(4) Uani 1 1 d . . . O16 O -0.3890(13) 0.9142(8) 0.8799(8) 0.076(4) Uani 1 1 d . . . O17 O -0.1723(16) 0.7331(8) 1.5908(8) 0.087(4) Uani 1 1 d . . . O18 O -0.2095(15) 0.8311(9) 0.9618(10) 0.102(5) Uani 1 1 d . . . O19 O -0.1605(14) 1.0189(8) 1.1445(10) 0.099(5) Uani 1 1 d . . . O20 O -0.3472(15) 1.1536(8) 1.2417(8) 0.078(4) Uani 1 1 d . . . O21 O 0.0413(12) 0.6526(7) 1.2444(7) 0.060(3) Uani 1 1 d . . . O22 O -0.0878(15) 0.7901(8) 1.1959(7) 0.072(3) Uani 1 1 d . . . O23 O 0.1035(14) 0.6689(9) 1.5125(9) 0.097(5) Uani 1 1 d . . . O24 O -0.4562(16) 0.7319(8) 0.8538(9) 0.088(4) Uani 1 1 d . . . O25 O 0.0518(15) 0.4757(7) 1.1513(7) 0.073(3) Uani 1 1 d . . . O26 O -0.3397(12) 0.7021(7) 1.4366(7) 0.062(3) Uani 1 1 d . . . O27 O -0.4066(14) 0.6875(9) 1.1795(9) 0.094(4) Uani 1 1 d . . . C1 C -0.3884(18) 0.5380(12) 1.2427(11) 0.073(5) Uani 1 1 d . . . H1A H -0.4048 0.5800 1.2984 0.109 Uiso 1 1 calc R . . H1B H -0.3824 0.4777 1.2413 0.109 Uiso 1 1 calc R . . H1C H -0.4818 0.5384 1.2056 0.109 Uiso 1 1 calc R . . C2 C -0.518(3) 0.8956(12) 1.1900(14) 0.102(7) Uani 1 1 d . . . H2A H -0.5276 0.8657 1.1303 0.153 Uiso 1 1 calc R . . H2B H -0.6264 0.8908 1.2109 0.153 Uiso 1 1 calc R . . H2C H -0.4364 0.8670 1.2124 0.153 Uiso 1 1 calc R . . C3 C 0.0936(18) 0.8162(12) 1.4448(11) 0.069(5) Uani 1 1 d . . . H3A H 0.1869 0.8113 1.4797 0.104 Uiso 1 1 calc R . . H3B H 0.0933 0.8779 1.4492 0.104 Uiso 1 1 calc R . . H3C H 0.1055 0.7759 1.3879 0.104 Uiso 1 1 calc R . . C4 C -0.498(2) 0.6847(13) 1.4707(13) 0.084(6) Uani 1 1 d . . . H4A H -0.4964 0.7250 1.5286 0.126 Uiso 1 1 calc R . . H4B H -0.5071 0.6225 1.4653 0.126 Uiso 1 1 calc R . . H4C H -0.5935 0.6953 1.4405 0.126 Uiso 1 1 calc R . . C5 C -0.215(2) 0.5300(11) 1.0408(12) 0.088(6) Uani 1 1 d . . . H5A H -0.2335 0.4939 1.0726 0.132 Uiso 1 1 calc R . . H5B H -0.1401 0.5007 0.9982 0.132 Uiso 1 1 calc R . . H5C H -0.3219 0.5359 1.0153 0.132 Uiso 1 1 calc R . . C6 C -0.108(3) 0.8240(13) 1.6554(13) 0.096(7) Uani 1 1 d . . . H6A H -0.0398 0.8157 1.6985 0.144 Uiso 1 1 calc R . . H6B H -0.2019 0.8587 1.6790 0.144 Uiso 1 1 calc R . . H6C H -0.0399 0.8561 1.6303 0.144 Uiso 1 1 calc R . . C7 C -0.168(3) 0.3951(15) 1.3142(13) 0.110(8) Uani 1 1 d . . . H7A H -0.0909 0.3655 1.3375 0.165 Uiso 1 1 calc R . . H7B H -0.2639 0.3532 1.2849 0.165 Uiso 1 1 calc R . . H7C H -0.2073 0.4473 1.3582 0.165 Uiso 1 1 calc R . . C8 C -0.131(2) 0.9566(12) 1.3685(12) 0.087(6) Uani 1 1 d . . . H8A H -0.0782 0.9047 1.3310 0.130 Uiso 1 1 calc R . . H8B H -0.0471 1.0068 1.3946 0.130 Uiso 1 1 calc R . . H8C H -0.2173 0.9735 1.3379 0.130 Uiso 1 1 calc R . . C9 C 0.1961(19) 0.6688(12) 1.2090(11) 0.072(5) Uani 1 1 d . . . H9A H 0.2924 0.6564 1.2375 0.108 Uiso 1 1 calc R . . H9B H 0.2070 0.7313 1.2155 0.108 Uiso 1 1 calc R . . H9C H 0.1908 0.6293 1.1508 0.108 Uiso 1 1 calc R . . C10 C -0.2398(19) 0.9746(12) 0.8883(13) 0.081(6) Uani 1 1 d . . . H10A H -0.2647 1.0368 0.9192 0.122 Uiso 1 1 calc R . . H10B H -0.2084 0.9674 0.8339 0.122 Uiso 1 1 calc R . . H10C H -0.1477 0.9596 0.9173 0.122 Uiso 1 1 calc R . . C11 C -0.369(2) 0.7104(14) 0.7767(12) 0.094(7) Uani 1 1 d . . . H11A H -0.3748 0.7601 0.7593 0.140 Uiso 1 1 calc R . . H11B H -0.4227 0.6558 0.7337 0.140 Uiso 1 1 calc R . . H11C H -0.2521 0.7013 0.7869 0.140 Uiso 1 1 calc R . . C12 C -0.269(3) 0.5510(14) 1.5575(12) 0.098(7) Uani 1 1 d . . . H12A H -0.1769 0.5334 1.5843 0.147 Uiso 1 1 calc R . . H12B H -0.3605 0.5041 1.5401 0.147 Uiso 1 1 calc R . . H12C H -0.3082 0.6071 1.5959 0.147 Uiso 1 1 calc R . . C13 C -0.376(3) 0.9725(12) 1.5787(14) 0.104(8) Uani 1 1 d . . . H13A H -0.3015 1.0098 1.5614 0.157 Uiso 1 1 calc R . . H13B H -0.3513 0.9873 1.6370 0.157 Uiso 1 1 calc R . . H13C H -0.4916 0.9836 1.5690 0.157 Uiso 1 1 calc R . . C14 C -0.811(2) 0.8055(13) 0.8925(15) 0.108(8) Uani 1 1 d . . . H14A H -0.9124 0.8339 0.8871 0.161 Uiso 1 1 calc R . . H14B H -0.8209 0.7819 0.9347 0.161 Uiso 1 1 calc R . . H14C H -0.7945 0.7564 0.8402 0.161 Uiso 1 1 calc R . . C15 C -0.381(2) 1.1736(14) 1.3273(11) 0.091(6) Uani 1 1 d . . . H15A H -0.5014 1.1763 1.3327 0.137 Uiso 1 1 calc R . . H15B H -0.3241 1.2313 1.3630 0.137 Uiso 1 1 calc R . . H15C H -0.3411 1.1265 1.3429 0.137 Uiso 1 1 calc R . . C16 C 0.085(3) 0.3829(12) 1.1114(13) 0.109(8) Uani 1 1 d . . . H16A H 0.2012 0.3756 1.1253 0.163 Uiso 1 1 calc R . . H16B H 0.0665 0.3634 1.0521 0.163 Uiso 1 1 calc R . . H16C H 0.0110 0.3465 1.1298 0.163 Uiso 1 1 calc R . . C17 C -0.055(3) 0.8000(13) 1.1227(12) 0.097(7) Uani 1 1 d . . . H17A H 0.0272 0.7587 1.0944 0.145 Uiso 1 1 calc R . . H17B H -0.0123 0.8616 1.1357 0.145 Uiso 1 1 calc R . . H17C H -0.1586 0.7865 1.0873 0.145 Uiso 1 1 calc R . . C18 C -0.555(3) 0.6756(12) 0.9767(14) 0.113(9) Uani 1 1 d . . . H18A H -0.4597 0.6465 0.9484 0.169 Uiso 1 1 calc R . . H18B H -0.6556 0.6554 0.9390 0.169 Uiso 1 1 calc R . . H18C H -0.5708 0.6597 1.0234 0.169 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 Re1 0.0435(4) 0.0297(4) 0.0334(5) 0.0133(3) 0.0065(3) 0.0056(3) Mo1 0.0435(4) 0.0297(4) 0.0334(5) 0.0133(3) 0.0065(3) 0.0056(3) Re2 0.0398(4) 0.0333(4) 0.0325(5) 0.0130(4) 0.0004(3) 0.0004(3) Mo2 0.0398(4) 0.0333(4) 0.0325(5) 0.0130(4) 0.0004(3) 0.0004(3) Re3 0.0403(4) 0.0292(4) 0.0281(4) 0.0139(3) 0.0035(3) 0.0041(3) Mo3 0.0403(4) 0.0292(4) 0.0281(4) 0.0139(3) 0.0035(3) 0.0041(3) Re4 0.0412(4) 0.0276(4) 0.0276(4) 0.0125(3) 0.0056(3) 0.0057(3) Mo4 0.0412(4) 0.0276(4) 0.0276(4) 0.0125(3) 0.0056(3) 0.0057(3) Re5 0.0429(4) 0.0298(4) 0.0259(5) 0.0118(3) 0.0043(3) 0.0023(3) Mo5 0.0429(4) 0.0298(4) 0.0259(5) 0.0118(3) 0.0043(3) 0.0023(3) Re6 0.0428(4) 0.0287(4) 0.0326(5) 0.0112(4) 0.0085(3) 0.0077(3) Mo6 0.0428(4) 0.0287(4) 0.0326(5) 0.0112(4) 0.0085(3) 0.0077(3) O1 0.075(7) 0.037(6) 0.104(10) 0.029(7) 0.003(7) -0.001(5) O2 0.067(7) 0.119(11) 0.115(11) 0.099(10) 0.012(7) 0.010(7) O3 0.059(6) 0.057(7) 0.063(8) 0.025(6) 0.002(6) 0.006(5) O4 0.083(7) 0.046(6) 0.081(9) 0.026(7) 0.013(7) 0.002(5) O5 0.093(8) 0.064(7) 0.062(8) 0.031(7) 0.004(7) 0.000(6) O6 0.093(8) 0.058(7) 0.065(8) 0.008(7) 0.009(7) -0.004(6) O7 0.067(7) 0.062(7) 0.103(11) 0.047(8) -0.012(7) -0.012(5) O8 0.098(9) 0.059(8) 0.088(10) 0.029(8) 0.026(8) 0.008(6) O9 0.092(9) 0.084(10) 0.085(10) 0.037(9) -0.009(8) 0.009(7) O10 0.034(7) 0.046(8) 0.072(11) 0.030(8) -0.006(7) 0.008(6) O11 0.100(9) 0.068(8) 0.055(8) 0.028(7) 0.017(7) 0.015(6) O12 0.077(8) 0.101(10) 0.110(12) 0.056(10) -0.010(8) 0.006(7) O13 0.067(6) 0.059(7) 0.078(9) 0.041(7) 0.019(6) 0.009(5) O14 0.094(8) 0.052(7) 0.062(8) 0.004(6) 0.023(7) 0.008(6) O15 0.098(9) 0.061(8) 0.082(10) 0.027(8) 0.007(8) -0.004(6) O16 0.056(6) 0.092(9) 0.111(11) 0.072(9) -0.002(7) 0.005(6) O17 0.116(10) 0.060(8) 0.066(9) 0.006(7) 0.014(8) -0.002(7) O18 0.071(8) 0.102(10) 0.132(13) 0.044(10) 0.005(8) 0.034(7) O19 0.069(8) 0.079(9) 0.146(14) 0.041(10) 0.006(8) 0.015(6) O20 0.093(9) 0.090(9) 0.065(9) 0.044(8) 0.009(7) 0.001(7) O21 0.065(6) 0.057(7) 0.068(8) 0.033(6) 0.017(6) 0.008(5) O22 0.095(8) 0.072(8) 0.055(8) 0.028(7) 0.009(7) 0.014(6) O23 0.076(8) 0.090(10) 0.138(14) 0.060(10) -0.018(8) 0.015(7) O24 0.105(9) 0.072(8) 0.106(11) 0.051(9) 0.044(9) 0.020(7) O25 0.104(9) 0.056(7) 0.056(8) 0.017(7) 0.022(7) 0.004(6) O26 0.058(6) 0.051(6) 0.071(8) 0.020(6) 0.003(6) 0.003(5) O27 0.070(7) 0.097(10) 0.126(13) 0.060(10) -0.023(8) 0.013(7) C1 0.056(10) 0.107(15) 0.069(13) 0.048(12) 0.017(9) 0.001(9) C2 0.127(17) 0.059(13) 0.11(2) 0.028(14) 0.001(15) 0.011(12) C3 0.058(10) 0.086(13) 0.057(12) 0.019(11) 0.024(9) 0.003(9) C4 0.060(10) 0.110(16) 0.108(17) 0.067(15) 0.036(11) 0.001(9) C5 0.125(16) 0.060(12) 0.066(13) 0.021(11) -0.042(12) -0.009(11) C6 0.134(18) 0.068(13) 0.079(16) 0.024(13) 0.007(14) 0.002(12) C7 0.142(19) 0.12(2) 0.091(18) 0.065(17) 0.052(16) 0.004(15) C8 0.109(15) 0.062(12) 0.088(16) 0.028(12) 0.031(13) 0.001(10) C9 0.067(10) 0.090(13) 0.074(13) 0.045(12) 0.037(10) 0.004(9) C10 0.057(10) 0.082(14) 0.110(18) 0.044(13) 0.010(11) -0.006(9) C11 0.107(15) 0.098(16) 0.064(13) 0.013(12) 0.053(12) 0.021(12) C12 0.133(18) 0.111(17) 0.080(15) 0.068(15) 0.037(14) -0.002(13) C13 0.142(19) 0.052(12) 0.109(19) 0.016(13) 0.051(16) 0.028(12) C14 0.065(12) 0.087(15) 0.19(3) 0.077(17) -0.016(14) -0.023(10) C15 0.109(16) 0.095(16) 0.054(13) 0.016(12) -0.009(12) -0.001(12) C16 0.16(2) 0.059(13) 0.082(16) -0.005(12) 0.048(16) 0.021(13) C17 0.17(2) 0.073(13) 0.069(14) 0.051(12) 0.041(15) 0.015(13) C18 0.17(2) 0.050(12) 0.13(2) 0.040(14) 0.083(18) 0.013(12) _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 Re1 O18 1.683(11) . ? Re1 O2 1.855(15) . ? Re1 O24 1.869(14) . ? Re1 O15 1.888(12) . ? Re1 O16 2.055(10) . ? Re1 O7 2.155(10) . ? Re2 O19 1.676(11) . ? Re2 O20 1.853(13) . ? Re2 O9 1.874(13) . ? Re2 O2 1.884(14) . ? Re2 O7 2.038(11) 2_477 ? Re2 O16 2.182(10) 2_477 ? Re3 O27 1.682(11) . ? Re3 O4 1.876(12) . ? Re3 O22 1.887(12) . ? Re3 O6 1.892(12) . ? Re3 O13 2.056(9) . ? Re3 O21 2.159(10) . ? Re4 O12 1.691(11) . ? Re4 O1 1.872(13) . ? Re4 O11 1.872(11) . ? Re4 O25 1.915(11) . ? Re4 O21 2.029(10) . ? Re4 O13 2.195(10) . ? Re5 O23 1.676(11) . ? Re5 O1 1.877(13) . ? Re5 O17 1.888(12) . ? Re5 O5 1.903(11) . ? Re5 O3 2.050(10) . ? Re5 O26 2.181(10) . ? Re6 O10 1.689(11) . ? Re6 O8 1.848(11) . ? Re6 O4 1.864(12) . ? Re6 O14 1.884(11) . ? Re6 O26 2.035(10) . ? Re6 O3 2.200(10) . ? O3 C3 1.443(16) . ? O5 C12 1.414(18) . ? O6 C5 1.437(18) . ? O7 C14 1.470(17) . ? O7 Mo2 2.038(11) 2_477 ? O7 Re2 2.038(11) 2_477 ? O8 C8 1.467(19) . ? O9 C2 1.49(2) . ? O11 C7 1.436(19) . ? O13 C1 1.447(16) . ? O14 C13 1.408(19) . ? O15 C18 1.432(18) . ? O16 C10 1.452(17) . ? O16 Mo2 2.182(10) 2_477 ? O16 Re2 2.182(10) 2_477 ? O17 C6 1.49(2) . ? O20 C15 1.45(2) . ? O21 C9 1.457(15) . ? O22 C17 1.388(18) . ? O24 C11 1.471(18) . ? O25 C16 1.413(19) . ? O26 C4 1.474(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 O18 Re1 O2 95.7(6) . . ? O18 Re1 O24 94.8(6) . . ? O2 Re1 O24 169.2(5) . . ? O18 Re1 O15 107.0(6) . . ? O2 Re1 O15 88.2(5) . . ? O24 Re1 O15 86.3(5) . . ? O18 Re1 O16 92.2(6) . . ? O2 Re1 O16 91.8(5) . . ? O24 Re1 O16 90.4(5) . . ? O15 Re1 O16 160.7(5) . . ? O18 Re1 O7 162.7(6) . . ? O2 Re1 O7 84.6(5) . . ? O24 Re1 O7 86.1(5) . . ? O15 Re1 O7 90.3(5) . . ? O16 Re1 O7 70.5(4) . . ? O19 Re2 O20 100.4(6) . . ? O19 Re2 O9 105.4(6) . . ? O20 Re2 O9 85.3(5) . . ? O19 Re2 O2 92.2(6) . . ? O20 Re2 O2 166.9(5) . . ? O9 Re2 O2 94.9(5) . . ? O19 Re2 O7 94.9(6) . 2_477 ? O20 Re2 O7 84.9(5) . 2_477 ? O9 Re2 O7 158.7(5) . 2_477 ? O2 Re2 O7 90.4(4) . 2_477 ? O19 Re2 O16 163.6(6) . 2_477 ? O20 Re2 O16 85.5(5) . 2_477 ? O9 Re2 O16 90.2(5) . 2_477 ? O2 Re2 O16 81.3(5) . 2_477 ? O7 Re2 O16 70.2(4) 2_477 2_477 ? O27 Re3 O4 95.4(6) . . ? O27 Re3 O22 107.4(5) . . ? O4 Re3 O22 89.7(5) . . ? O27 Re3 O6 95.8(6) . . ? O4 Re3 O6 168.8(5) . . ? O22 Re3 O6 87.0(5) . . ? O27 Re3 O13 92.3(5) . . ? O4 Re3 O13 92.8(4) . . ? O22 Re3 O13 159.8(4) . . ? O6 Re3 O13 86.7(5) . . ? O27 Re3 O21 162.6(5) . . ? O4 Re3 O21 83.5(4) . . ? O22 Re3 O21 89.9(4) . . ? O6 Re3 O21 85.8(5) . . ? O13 Re3 O21 70.5(4) . . ? O12 Re4 O1 92.9(6) . . ? O12 Re4 O11 104.5(5) . . ? O1 Re4 O11 93.5(5) . . ? O12 Re4 O25 100.0(6) . . ? O1 Re4 O25 166.9(5) . . ? O11 Re4 O25 85.5(5) . . ? O12 Re4 O21 95.3(5) . . ? O1 Re4 O21 92.0(4) . . ? O11 Re4 O21 159.2(5) . . ? O25 Re4 O21 84.5(4) . . ? O12 Re4 O13 164.6(5) . . ? O1 Re4 O13 82.7(4) . . ? O11 Re4 O13 90.6(4) . . ? O25 Re4 O13 84.3(5) . . ? O21 Re4 O13 70.2(4) . . ? O23 Re5 O1 95.3(6) . . ? O23 Re5 O17 96.5(7) . . ? O1 Re5 O17 168.0(5) . . ? O23 Re5 O5 106.1(5) . . ? O1 Re5 O5 88.4(5) . . ? O17 Re5 O5 86.3(5) . . ? O23 Re5 O3 93.0(5) . . ? O1 Re5 O3 92.5(4) . . ? O17 Re5 O3 89.1(5) . . ? O5 Re5 O3 160.7(4) . . ? O23 Re5 O26 163.7(5) . . ? O1 Re5 O26 82.9(4) . . ? O17 Re5 O26 86.3(5) . . ? O5 Re5 O26 90.0(4) . . ? O3 Re5 O26 71.0(4) . . ? O10 Re6 O8 104.4(6) . . ? O10 Re6 O4 92.4(6) . . ? O8 Re6 O4 95.2(5) . . ? O10 Re6 O14 100.2(6) . . ? O8 Re6 O14 85.2(5) . . ? O4 Re6 O14 166.8(5) . . ? O10 Re6 O26 94.9(5) . . ? O8 Re6 O26 159.9(5) . . ? O4 Re6 O26 89.3(4) . . ? O14 Re6 O26 86.0(5) . . ? O10 Re6 O3 164.6(5) . . ? O8 Re6 O3 90.4(5) . . ? O4 Re6 O3 81.8(4) . . ? O14 Re6 O3 85.0(5) . . ? O26 Re6 O3 70.8(4) . . ? Re4 O1 Re5 163.0(6) . . ? Re1 O2 Re2 162.0(6) . . ? C3 O3 Re5 121.2(9) . . ? C3 O3 Re6 118.3(9) . . ? Re5 O3 Re6 108.4(4) . . ? Re6 O4 Re3 159.5(7) . . ? C12 O5 Re5 128.3(12) . . ? C5 O6 Re3 125.6(11) . . ? C14 O7 Mo2 119.1(11) . 2_477 ? C14 O7 Re2 119.1(11) . 2_477 ? Mo2 O7 Re2 0.00(3) 2_477 2_477 ? C14 O7 Re1 119.8(9) . . ? Mo2 O7 Re1 110.4(5) 2_477 . ? Re2 O7 Re1 110.4(5) 2_477 . ? C8 O8 Re6 127.0(11) . . ? C2 O9 Re2 125.6(12) . . ? C7 O11 Re4 132.9(12) . . ? C1 O13 Re3 121.7(9) . . ? C1 O13 Re4 118.6(9) . . ? Re3 O13 Re4 108.2(4) . . ? C13 O14 Re6 129.2(12) . . ? C18 O15 Re1 127.8(12) . . ? C10 O16 Re1 124.0(10) . . ? C10 O16 Mo2 118.4(9) . 2_477 ? Re1 O16 Mo2 108.7(5) . 2_477 ? C10 O16 Re2 118.4(9) . 2_477 ? Re1 O16 Re2 108.7(5) . 2_477 ? Mo2 O16 Re2 0.000(15) 2_477 2_477 ? C6 O17 Re5 129.4(11) . . ? C15 O20 Re2 131.7(11) . . ? C9 O21 Re4 119.0(9) . . ? C9 O21 Re3 119.8(9) . . ? Re4 O21 Re3 110.7(4) . . ? C17 O22 Re3 126.6(12) . . ? C11 O24 Re1 126.1(11) . . ? C16 O25 Re4 125.7(12) . . ? C4 O26 Re6 118.9(9) . . ? C4 O26 Re5 118.4(9) . . ? Re6 O26 Re5 109.7(4) . . ? _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.858 _refine_diff_density_max 2.331 _refine_diff_density_min -2.467 _refine_diff_density_rms 0.313 #========================================================================== #======================================================================= #Compound 5 data_renb10m _database_code_CSD 152229 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H42 Nb4 O24 Re2' _chemical_formula_weight 1338.52 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' 'Nb' 'Nb' -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.716(4) _cell_length_b 15.888(7) _cell_length_c 12.128(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.059(9) _cell_angle_gamma 90.00 _cell_volume 1837.5(14) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 999 (I>10sigma(I)( _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 28.47 _exptl_crystal_description plate _exptl_crystal_colour light pink _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.419 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 7.846 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker SMART CCD 1K' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10870 _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_sigmaI/netI 0.0743 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 28.47 _reflns_number_total 4247 _reflns_number_gt 2243 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.0895P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4247 _refine_ls_number_parameters 201 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1016 _refine_ls_R_factor_gt 0.0552 _refine_ls_wR_factor_ref 0.1564 _refine_ls_wR_factor_gt 0.1422 _refine_ls_goodness_of_fit_ref 0.875 _refine_ls_restrained_S_all 0.875 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.20969(7) 0.13780(4) 0.06814(5) 0.0918(3) Uani 1 1 d . . . Nb2 Nb 0.31733(8) 0.02461(5) 0.34276(8) 0.0487(3) Uani 1 1 d . . . Nb3 Nb 0.66448(9) 0.07172(6) 0.36684(8) 0.0532(3) Uani 1 1 d . . . O1 O 0.2272(7) -0.0656(5) 0.2634(7) 0.070(2) Uani 1 1 d . . . O2 O 0.5113(6) -0.0202(4) 0.3160(6) 0.0509(15) Uani 1 1 d . . . O3 O 0.4669(6) 0.1197(4) 0.3790(6) 0.0506(16) Uani 1 1 d . . . O4 O 0.3396(6) -0.0204(4) 0.4795(6) 0.0561(17) Uani 1 1 d . . . O5 O 0.3083(8) 0.0781(5) 0.1710(7) 0.079(2) Uani 1 1 d . . . O6 O 0.7508(7) 0.1662(5) 0.4382(7) 0.072(2) Uani 1 1 d . . . O7 O 0.1729(7) 0.0985(4) 0.3507(7) 0.069(2) Uani 1 1 d . . . O8 O 0.8055(7) 0.0004(5) 0.3555(7) 0.072(2) Uani 1 1 d . . . O9 O 0.6434(9) 0.1119(5) 0.2216(8) 0.078(2) Uani 1 1 d . . . O11 O 0.0356(12) 0.1108(12) 0.0560(16) 0.209(8) Uani 1 1 d . . . O12 O 0.2296(17) 0.2383(7) 0.0965(11) 0.155(6) Uani 1 1 d . . . C1 C 0.4379(12) 0.2085(7) 0.3743(13) 0.086(4) Uani 1 1 d . . . H1A H 0.3763 0.2219 0.4249 0.129 Uiso 1 1 calc R . . H1B H 0.3939 0.2237 0.2991 0.129 Uiso 1 1 calc R . . H1C H 0.5240 0.2392 0.3955 0.129 Uiso 1 1 calc R . . C2 C 0.5409(13) -0.1077(7) 0.3113(15) 0.095(5) Uani 1 1 d . . . H2A H 0.5641 -0.1208 0.2398 0.143 Uiso 1 1 calc R . . H2B H 0.4601 -0.1395 0.3209 0.143 Uiso 1 1 calc R . . H2C H 0.6187 -0.1217 0.3701 0.143 Uiso 1 1 calc R . . C3 C 0.7966(17) 0.2108(9) 0.5370(12) 0.099(5) Uani 1 1 d . . . H3A H 0.7382 0.1974 0.5901 0.148 Uiso 1 1 calc R . . H3B H 0.7913 0.2700 0.5213 0.148 Uiso 1 1 calc R . . H3C H 0.8919 0.1956 0.5677 0.148 Uiso 1 1 calc R . . C4 C 0.0694(13) 0.1600(8) 0.3413(13) 0.089(4) Uani 1 1 d . . . H4A H 0.0988 0.2090 0.3056 0.134 Uiso 1 1 calc R . . H4B H 0.0541 0.1748 0.4148 0.134 Uiso 1 1 calc R . . H4C H -0.0162 0.1388 0.2971 0.134 Uiso 1 1 calc R . . C5 C 0.1793(19) -0.1049(12) 0.1648(14) 0.133(7) Uani 1 1 d . . . H5A H 0.0875 -0.0841 0.1329 0.199 Uiso 1 1 calc R . . H5B H 0.1744 -0.1644 0.1775 0.199 Uiso 1 1 calc R . . H5C H 0.2418 -0.0942 0.1140 0.199 Uiso 1 1 calc R . . C6 C 0.6302(18) 0.0858(11) 0.1130(14) 0.112(5) Uani 1 1 d . . . H6A H 0.7215 0.0758 0.0964 0.169 Uiso 1 1 calc R . . H6B H 0.5833 0.1285 0.0636 0.169 Uiso 1 1 calc R . . H6C H 0.5765 0.0347 0.1025 0.169 Uiso 1 1 calc R . . C7 C 0.9058(14) -0.0624(9) 0.3525(19) 0.143(8) Uani 1 1 d . . . H7A H 0.9803 -0.0568 0.4167 0.215 Uiso 1 1 calc R . . H7B H 0.9431 -0.0567 0.2851 0.215 Uiso 1 1 calc R . . H7C H 0.8628 -0.1167 0.3536 0.215 Uiso 1 1 calc R . . O10 O 0.2594(15) 0.1157(9) -0.0390(13) 0.157(5) Uiso 1 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 Re1 0.1243(5) 0.0735(4) 0.0642(4) 0.0084(3) -0.0154(3) 0.0061(3) Nb2 0.0378(4) 0.0534(5) 0.0528(6) 0.0016(4) 0.0032(3) -0.0015(4) Nb3 0.0431(4) 0.0560(5) 0.0629(6) 0.0038(5) 0.0155(4) -0.0053(4) O1 0.057(4) 0.072(5) 0.073(6) -0.008(4) -0.005(4) -0.013(4) O2 0.051(3) 0.049(4) 0.052(4) -0.003(3) 0.009(3) 0.003(3) O3 0.040(3) 0.047(4) 0.063(5) -0.001(3) 0.004(3) 0.002(3) O4 0.047(3) 0.065(5) 0.056(4) -0.001(3) 0.010(3) -0.005(3) O5 0.060(4) 0.100(6) 0.070(5) 0.024(5) -0.002(4) -0.002(4) O6 0.057(4) 0.064(5) 0.094(7) 0.003(4) 0.015(4) -0.023(4) O7 0.044(3) 0.062(4) 0.098(6) -0.001(4) 0.006(4) 0.008(3) O8 0.047(4) 0.076(5) 0.099(6) -0.003(4) 0.029(4) 0.002(4) O9 0.081(5) 0.084(6) 0.075(6) 0.005(5) 0.028(5) -0.007(4) O11 0.075(7) 0.272(18) 0.237(17) -0.043(14) -0.080(9) 0.006(9) O12 0.256(17) 0.077(7) 0.121(10) 0.004(6) 0.007(10) 0.014(8) C1 0.067(7) 0.053(7) 0.131(12) -0.011(7) 0.003(7) 0.007(5) C2 0.067(7) 0.057(7) 0.164(15) -0.022(8) 0.029(9) 0.002(6) C3 0.118(11) 0.076(9) 0.097(12) -0.010(8) 0.009(9) -0.025(8) C4 0.067(7) 0.079(8) 0.122(13) -0.008(8) 0.019(8) 0.016(6) C5 0.157(16) 0.160(16) 0.080(12) -0.047(11) 0.021(11) -0.060(14) C6 0.131(13) 0.117(13) 0.093(13) 0.025(10) 0.031(10) -0.014(11) C7 0.063(8) 0.078(10) 0.29(3) -0.026(13) 0.028(12) 0.009(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 Re1 O10 1.512(16) . ? Re1 O12 1.638(11) . ? Re1 O5 1.707(8) . ? Re1 O11 1.724(13) . ? Nb2 O4 1.780(7) . ? Nb2 O7 1.846(7) . ? Nb2 O1 1.850(7) . ? Nb2 O3 2.084(6) . ? Nb2 O2 2.097(6) . ? Nb2 O5 2.236(8) . ? Nb3 O8 1.804(7) . ? Nb3 O9 1.848(9) . ? Nb3 O6 1.852(8) . ? Nb3 O4 2.042(7) 3_656 ? Nb3 O2 2.093(6) . ? Nb3 O3 2.097(6) . ? O1 C5 1.351(15) . ? O2 C2 1.422(12) . ? O3 C1 1.438(12) . ? O4 Nb3 2.042(7) 3_656 ? O6 C3 1.389(15) . ? O7 C4 1.392(13) . ? O8 C7 1.399(14) . ? O9 C6 1.364(17) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 Re1 O12 111.3(7) . . ? O10 Re1 O5 105.8(6) . . ? O12 Re1 O5 111.2(6) . . ? O10 Re1 O11 109.8(8) . . ? O12 Re1 O11 109.6(8) . . ? O5 Re1 O11 109.2(7) . . ? O4 Nb2 O7 99.5(3) . . ? O4 Nb2 O1 97.7(3) . . ? O7 Nb2 O1 103.3(3) . . ? O4 Nb2 O3 98.0(3) . . ? O7 Nb2 O3 92.0(3) . . ? O1 Nb2 O3 155.9(3) . . ? O4 Nb2 O2 93.2(3) . . ? O7 Nb2 O2 159.8(3) . . ? O1 Nb2 O2 90.4(3) . . ? O3 Nb2 O2 70.6(2) . . ? O4 Nb2 O5 175.1(3) . . ? O7 Nb2 O5 85.0(3) . . ? O1 Nb2 O5 83.1(3) . . ? O3 Nb2 O5 79.8(3) . . ? O2 Nb2 O5 82.0(3) . . ? O8 Nb3 O9 95.3(4) . . ? O8 Nb3 O6 105.2(4) . . ? O9 Nb3 O6 97.0(4) . . ? O8 Nb3 O4 88.1(3) . 3_656 ? O9 Nb3 O4 172.0(3) . 3_656 ? O6 Nb3 O4 89.1(3) . 3_656 ? O8 Nb3 O2 92.7(3) . . ? O9 Nb3 O2 91.0(3) . . ? O6 Nb3 O2 159.5(3) . . ? O4 Nb3 O2 81.5(3) 3_656 . ? O8 Nb3 O3 162.4(3) . . ? O9 Nb3 O3 90.3(3) . . ? O6 Nb3 O3 90.6(3) . . ? O4 Nb3 O3 84.4(3) 3_656 . ? O2 Nb3 O3 70.4(2) . . ? C5 O1 Nb2 150.1(10) . . ? C2 O2 Nb3 123.7(6) . . ? C2 O2 Nb2 122.2(6) . . ? Nb3 O2 Nb2 109.1(3) . . ? C1 O3 Nb2 125.4(6) . . ? C1 O3 Nb3 121.9(6) . . ? Nb2 O3 Nb3 109.4(3) . . ? Nb2 O4 Nb3 172.1(4) . 3_656 ? Re1 O5 Nb2 143.9(5) . . ? C3 O6 Nb3 149.1(8) . . ? C4 O7 Nb2 170.8(9) . . ? C7 O8 Nb3 173.0(9) . . ? C6 O9 Nb3 142.0(9) . . ? _diffrn_measured_fraction_theta_max 0.916 _diffrn_reflns_theta_full 28.47 _diffrn_measured_fraction_theta_full 0.916 _refine_diff_density_max 2.950 _refine_diff_density_min -2.846 _refine_diff_density_rms 0.176 #========================================================================== #======================================================================= #Compound 6 data_reta0m _database_code_CSD 152230 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H42 O24 Re2 Ta4' _chemical_formula_weight 1690.68 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' 'Ta' 'Ta' -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Re' 'Re' -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.8256(17) _cell_length_b 15.938(3) _cell_length_c 12.265(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.344(3) _cell_angle_gamma 90.00 _cell_volume 1883.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 999(I>4sigma(I)) _cell_measurement_theta_min 2.12 _cell_measurement_theta_max 22.50 _exptl_crystal_description prism _exptl_crystal_colour light pink _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.982 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 18.051 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.0360 _exptl_absorpt_correction_T_max 0.1229 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7487 _diffrn_reflns_av_R_equivalents 0.1093 _diffrn_reflns_av_sigmaI/netI 0.1004 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 22.50 _reflns_number_total 2450 _reflns_number_gt 1458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w==1/[\s^2^(Fo^2^)+(0.1000P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2450 _refine_ls_number_parameters 206 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1122 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.1698 _refine_ls_wR_factor_gt 0.1548 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.926 _refine_ls_shift/su_max 1.248 _refine_ls_shift/su_mean 0.029 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 Ta1 Ta 0.18137(10) 0.02412(8) 0.16065(9) 0.0556(4) Uani 1 1 d . . . Ta2 Ta 0.16564(10) -0.06821(8) -0.12921(10) 0.0610(4) Uani 1 1 d . . . Re1 Re 0.2806(2) 0.13775(12) 0.43129(13) 0.1106(7) Uani 1 1 d . . . O7 O 0.1645(14) -0.0195(12) 0.0250(16) 0.077(6) Uani 1 1 d . . . O10 O -0.0148(15) -0.0183(12) 0.1827(13) 0.058(5) Uani 1 1 d . . . O11 O 0.192(2) 0.0769(15) 0.3316(16) 0.092(7) Uani 1 1 d . . . O13 O 0.2746(16) -0.0644(12) 0.2378(15) 0.072(5) Uani 1 1 d . . . O22 O 0.0348(14) 0.1157(12) 0.1213(14) 0.065(5) Uani 1 1 d . . . O1 O 0.3051(18) 0.0067(14) -0.1416(17) 0.091(7) Uani 1 1 d . . . O2 O 0.2535(16) -0.1632(13) -0.0629(17) 0.080(6) Uani 1 1 d . . . O3 O 0.150(2) -0.1061(16) -0.268(2) 0.114(8) Uani 1 1 d . . . O4 O 0.3229(17) 0.0960(13) 0.1579(17) 0.085(6) Uani 1 1 d . . . C1 C 0.302(3) -0.2101(19) 0.035(3) 0.085(10) Uani 1 1 d . . . H1A H 0.2885 -0.1784 0.0984 0.127 Uiso 1 1 calc R . . H1B H 0.3989 -0.2220 0.0409 0.127 Uiso 1 1 calc R . . H1C H 0.2511 -0.2618 0.0315 0.127 Uiso 1 1 calc R . . C2 C 0.126(5) -0.085(3) -0.389(2) 0.146(19) Uani 1 1 d . . . H2A H 0.0544 -0.0430 -0.4058 0.220 Uiso 1 1 calc R . . H2B H 0.0988 -0.1340 -0.4326 0.220 Uiso 1 1 calc R . . H2C H 0.2105 -0.0627 -0.4066 0.220 Uiso 1 1 calc R . . C3 C 0.058(3) 0.206(2) 0.117(3) 0.095(11) Uani 1 1 d . . . H3A H -0.0136 0.2350 0.1447 0.142 Uiso 1 1 calc R . . H3B H 0.0556 0.2223 0.0411 0.142 Uiso 1 1 calc R . . H3C H 0.1467 0.2195 0.1613 0.142 Uiso 1 1 calc R . . C4 C -0.035(3) -0.107(2) 0.199(4) 0.127(17) Uani 1 1 d . . . H4A H -0.1314 -0.1175 0.1984 0.191 Uiso 1 1 calc R . . H4B H 0.0193 -0.1238 0.2696 0.191 Uiso 1 1 calc R . . H4C H -0.0065 -0.1382 0.1408 0.191 Uiso 1 1 calc R . . O110 O 0.228(4) 0.113(2) 0.509(5) 0.22(2) Uani 1 1 d . . . O111 O 0.258(4) 0.237(2) 0.398(3) 0.190(14) Uani 1 1 d . . . C5 C 0.327(5) -0.109(3) 0.333(4) 0.19(3) Uani 1 1 d . . . H5A H 0.3743 -0.0710 0.3893 0.278 Uiso 1 1 calc R . . H5B H 0.3916 -0.1502 0.3175 0.278 Uiso 1 1 calc R . . H5C H 0.2528 -0.1359 0.3597 0.278 Uiso 1 1 calc R . . C6 C 0.423(4) 0.164(3) 0.164(4) 0.135(16) Uani 1 1 d . . . H6A H 0.4457 0.1725 0.0924 0.203 Uiso 1 1 calc R . . H6B H 0.5054 0.1499 0.2171 0.203 Uiso 1 1 calc R . . H6C H 0.3835 0.2146 0.1873 0.203 Uiso 1 1 calc R . . O116 O 0.453(4) 0.121(3) 0.455(4) 0.27(3) Uani 1 1 d . . . C7 C 0.406(4) 0.061(3) -0.163(5) 0.21(3) Uani 1 1 d . . . H7A H 0.3951 0.0691 -0.2415 0.315 Uiso 1 1 calc R . . H7B H 0.4959 0.0375 -0.1340 0.315 Uiso 1 1 calc R . . H7C H 0.3971 0.1137 -0.1273 0.315 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 Ta1 0.0323(6) 0.0786(9) 0.0511(7) -0.0025(6) -0.0037(5) 0.0006(5) Ta2 0.0369(6) 0.0802(9) 0.0667(8) -0.0074(7) 0.0117(5) 0.0043(5) Re1 0.1437(17) 0.1026(13) 0.0673(10) -0.0123(9) -0.0237(10) -0.0036(11) O7 0.021(8) 0.102(15) 0.112(16) 0.041(13) 0.020(9) 0.016(9) O10 0.045(10) 0.079(13) 0.047(10) 0.014(9) 0.004(8) -0.029(9) O11 0.076(13) 0.13(2) 0.059(12) -0.014(13) -0.012(10) 0.019(13) O13 0.033(9) 0.092(14) 0.084(13) -0.001(12) -0.008(9) 0.031(9) O22 0.026(8) 0.092(15) 0.068(12) 0.013(11) -0.015(8) -0.021(9) O1 0.053(12) 0.115(18) 0.102(17) 0.022(13) 0.010(11) -0.031(11) O2 0.041(10) 0.100(16) 0.095(15) 0.011(13) 0.001(10) 0.037(10) O3 0.093(16) 0.111(19) 0.15(2) -0.005(16) 0.043(16) 0.033(14) O4 0.046(11) 0.093(16) 0.106(16) -0.006(12) -0.013(11) -0.032(10) C1 0.09(2) 0.07(2) 0.09(2) -0.030(19) 0.00(2) 0.007(17) C2 0.27(6) 0.15(4) 0.026(17) -0.02(2) 0.04(3) 0.00(4) C3 0.042(16) 0.12(3) 0.11(3) 0.01(2) -0.017(17) -0.021(17) C4 0.032(16) 0.08(2) 0.26(5) 0.04(3) 0.01(2) -0.006(15) O110 0.17(3) 0.11(3) 0.44(6) 0.02(3) 0.19(4) -0.07(2) O111 0.23(4) 0.16(3) 0.16(3) 0.07(2) -0.01(3) 0.04(3) C5 0.19(5) 0.18(4) 0.14(4) -0.03(3) -0.09(4) 0.14(4) C6 0.08(3) 0.14(4) 0.19(5) 0.01(3) 0.04(3) -0.01(2) O116 0.15(3) 0.26(4) 0.31(5) -0.03(4) -0.18(3) 0.08(3) C7 0.07(3) 0.19(5) 0.35(8) 0.10(5) -0.04(4) -0.06(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 O7 1.78(2) . ? Ta1 O4 1.807(17) . ? Ta1 O13 1.840(17) . ? Ta1 O22 2.040(18) . ? Ta1 O10 2.109(14) . ? Ta1 O11 2.24(2) . ? Ta2 O3 1.78(3) . ? Ta2 O1 1.847(18) . ? Ta2 O2 1.850(18) . ? Ta2 O10 2.036(18) 3 ? Ta2 O7 2.05(2) . ? Ta2 O22 2.130(15) 3 ? Re1 O110 1.23(4) . ? Re1 O111 1.64(3) . ? Re1 O11 1.67(2) . ? Re1 O116 1.68(3) . ? O10 C4 1.45(3) . ? O10 Ta2 2.036(18) 3 ? O13 C5 1.38(4) . ? O22 C3 1.46(3) . ? O22 Ta2 2.130(15) 3 ? O1 C7 1.38(4) . ? O2 C1 1.41(3) . ? O3 C2 1.50(4) . ? O4 C6 1.45(4) . ? 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 O7 Ta1 O4 99.3(9) . . ? O7 Ta1 O13 97.3(8) . . ? O4 Ta1 O13 100.9(9) . . ? O7 Ta1 O22 97.3(7) . . ? O4 Ta1 O22 93.0(8) . . ? O13 Ta1 O22 158.0(7) . . ? O7 Ta1 O10 94.3(7) . . ? O4 Ta1 O10 158.6(9) . . ? O13 Ta1 O10 93.6(7) . . ? O22 Ta1 O10 68.9(7) . . ? O7 Ta1 O11 177.2(7) . . ? O4 Ta1 O11 83.3(9) . . ? O13 Ta1 O11 83.1(8) . . ? O22 Ta1 O11 81.6(7) . . ? O10 Ta1 O11 82.9(7) . . ? O3 Ta2 O1 93.9(11) . . ? O3 Ta2 O2 95.0(10) . . ? O1 Ta2 O2 106.0(9) . . ? O3 Ta2 O10 90.0(9) . 3 ? O1 Ta2 O10 92.3(8) . 3 ? O2 Ta2 O10 160.6(7) . 3 ? O3 Ta2 O7 174.2(8) . . ? O1 Ta2 O7 88.3(8) . . ? O2 Ta2 O7 89.5(8) . . ? O10 Ta2 O7 84.5(6) 3 . ? O3 Ta2 O22 90.8(9) . 3 ? O1 Ta2 O22 160.3(9) . 3 ? O2 Ta2 O22 92.6(8) . 3 ? O10 Ta2 O22 68.5(7) 3 3 ? O7 Ta2 O22 85.4(6) . 3 ? O110 Re1 O111 116(2) . . ? O110 Re1 O11 98(2) . . ? O111 Re1 O11 110.8(16) . . ? O110 Re1 O116 112(3) . . ? O111 Re1 O116 106(2) . . ? O11 Re1 O116 113.3(16) . . ? Ta1 O7 Ta2 174.4(8) . . ? C4 O10 Ta2 126.5(14) . 3 ? C4 O10 Ta1 119.0(15) . . ? Ta2 O10 Ta1 111.6(8) 3 . ? Re1 O11 Ta1 145.8(13) . . ? C5 O13 Ta1 154(2) . . ? C3 O22 Ta1 127.4(14) . . ? C3 O22 Ta2 120.3(15) . 3 ? Ta1 O22 Ta2 110.5(8) . 3 ? C7 O1 Ta2 174(3) . . ? C1 O2 Ta2 148.8(18) . . ? C2 O3 Ta2 147(2) . . ? C6 O4 Ta1 170(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.988 _refine_diff_density_min -2.924 _refine_diff_density_rms 0.329