# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Martinez-Lillo, Jose' _publ_contact_author_email lillo@uv.es _publ_section_title ; Synthesis, crystal structure and magnetic properties of an oxalato-bridged ReIVMoVI heterobimetallic complex ; loop_ _publ_author_name J.Martinez-Lillo D.Armentano 'De Munno' F.Lloret M.Julve J.Faus # Attachment '- CIF_1.CIF' data_Compound1 _database_code_depnum_ccdc_archive 'CCDC 795006' #TrackingRef '- CIF_1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H40 Cl6 Mo O6 P2 Re' _chemical_formula_weight 1293.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.6472(4) _cell_length_b 11.7440(5) _cell_length_c 11.9908(5) _cell_angle_alpha 101.132(2) _cell_angle_beta 93.506(2) _cell_angle_gamma 106.2570(10) _cell_volume 1270.05(9) _cell_formula_units_Z 1 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7175 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.02 _exptl_crystal_description IRREGULAR _exptl_crystal_colour bronze _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 637 _exptl_absorpt_coefficient_mu 3.054 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.5803 _exptl_absorpt_correction_T_max 0.8380 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15176 _diffrn_reflns_av_R_equivalents 0.0130 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 31.25 _reflns_number_total 12010 _reflns_number_gt 10397 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius SAINT' _computing_cell_refinement 'Bruker-Nonius SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1339P)^2^+2.9014P] 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 RIDING _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.741(10) _refine_ls_number_reflns 12010 _refine_ls_number_parameters 591 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0822 _refine_ls_wR_factor_ref 0.2193 _refine_ls_wR_factor_gt 0.2128 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Re1 Re 0.99092(3) -0.24164(3) 0.99012(3) 0.05123(14) Uani 1 1 d . . . Mo1 Mo 1.00637(14) 0.24264(14) 1.00824(9) 0.0647(4) Uani 1 1 d . . . Cl1 Cl 1.0313(7) -0.2542(5) 0.7980(4) 0.0714(12) Uani 1 1 d . . . Cl2 Cl 1.1649(7) -0.3282(5) 1.0280(4) 0.0774(14) Uani 1 1 d . . . Cl3 Cl 0.9475(8) -0.2096(6) 1.1811(5) 0.0800(15) Uani 1 1 d . . . Cl4 Cl 0.8082(8) -0.4187(5) 0.9457(6) 0.0948(19) Uani 1 1 d . . . Cl5 Cl 1.0422(5) 0.1797(4) 0.8139(4) 0.0746(10) Uani 1 1 d . . . Cl6 Cl 0.9697(8) 0.2343(5) 1.1975(5) 0.0931(15) Uani 1 1 d . . . C1 C 1.0778(12) 0.0121(9) 1.0205(11) 0.043(2) Uani 1 1 d . . . C2 C 0.9165(13) -0.0282(12) 0.9843(11) 0.052(3) Uani 1 1 d . . . O1 O 1.1399(12) -0.0665(10) 1.0308(13) 0.059(3) Uani 1 1 d . . . O2 O 0.8502(12) -0.1388(8) 0.9654(10) 0.049(2) Uani 1 1 d . . . O3 O 0.8583(11) 0.0519(9) 0.9765(11) 0.062(3) Uani 1 1 d . . . O4 O 1.1428(10) 0.1216(9) 1.0386(10) 0.062(3) Uani 1 1 d . . . O5 O 1.1613(11) 0.3737(7) 1.0392(11) 0.074(3) Uani 1 1 d . . . O6 O 0.8536(14) 0.2965(11) 0.9744(11) 0.077(3) Uiso 1 1 d . . . P1 P 0.4713(3) 0.7469(2) 0.6282(2) 0.0400(5) Uani 1 1 d . . . C3 C 0.4505(11) 0.8829(9) 0.7132(11) 0.045(2) Uani 1 1 d . . . C4 C 0.3463(15) 0.9368(13) 0.6749(14) 0.060(3) Uani 1 1 d . . . H4A H 0.2847 0.8999 0.6070 0.072 Uiso 1 1 calc R . . C5 C 0.339(2) 1.0425(15) 0.739(2) 0.080(5) Uani 1 1 d . . . H5B H 0.2779 1.0817 0.7104 0.096 Uiso 1 1 calc R . . C6 C 0.416(2) 1.0932(14) 0.8428(18) 0.075(5) Uani 1 1 d . . . H6B H 0.3996 1.1602 0.8889 0.089 Uiso 1 1 calc R . . C7 C 0.5238(19) 1.0437(14) 0.8808(14) 0.068(4) Uani 1 1 d . . . H7A H 0.5867 1.0840 0.9475 0.081 Uiso 1 1 calc R . . C8 C 0.5345(18) 0.9359(14) 0.8189(13) 0.061(3) Uani 1 1 d . . . H8A H 0.5977 0.8984 0.8475 0.073 Uiso 1 1 calc R . . C9 C 0.3371(10) 0.6901(11) 0.5046(10) 0.043(2) Uani 1 1 d . . . C10 C 0.2265(14) 0.5799(11) 0.4942(13) 0.055(3) Uani 1 1 d . . . H10A H 0.2194 0.5369 0.5522 0.066 Uiso 1 1 calc R . . C11 C 0.1272(15) 0.5364(15) 0.3939(15) 0.066(4) Uani 1 1 d . . . H11A H 0.0564 0.4615 0.3830 0.079 Uiso 1 1 calc R . . C12 C 0.1343(18) 0.6019(16) 0.3149(17) 0.070(4) Uani 1 1 d . . . H12A H 0.0646 0.5727 0.2509 0.084 Uiso 1 1 calc R . . C13 C 0.2400(18) 0.7113(18) 0.3227(13) 0.069(4) Uani 1 1 d . . . H13A H 0.2422 0.7533 0.2642 0.083 Uiso 1 1 calc R . . C14 C 0.3439(16) 0.7584(14) 0.4200(15) 0.052(4) Uani 1 1 d . . . H14A H 0.4152 0.8325 0.4281 0.063 Uiso 1 1 calc R . . C15 C 0.6476(13) 0.7781(13) 0.5753(11) 0.040(2) Uani 1 1 d . . . C16 C 0.6603(13) 0.6927(11) 0.4793(11) 0.052(3) Uani 1 1 d . . . H16A H 0.5803 0.6286 0.4420 0.062 Uiso 1 1 calc R . . C17 C 0.7970(16) 0.7079(14) 0.4427(14) 0.064(3) Uani 1 1 d . . . H17A H 0.8078 0.6542 0.3782 0.076 Uiso 1 1 calc R . . C18 C 0.9141(14) 0.7984(13) 0.4981(14) 0.061(3) Uani 1 1 d . . . H18A H 1.0050 0.8048 0.4737 0.073 Uiso 1 1 calc R . . C19 C 0.8996(13) 0.8801(15) 0.5893(14) 0.064(4) Uani 1 1 d . . . H19A H 0.9804 0.9444 0.6248 0.077 Uiso 1 1 calc R . . C20 C 0.7639(14) 0.8701(13) 0.6323(12) 0.054(3) Uani 1 1 d . . . H20A H 0.7551 0.9245 0.6971 0.065 Uiso 1 1 calc R . . C21 C 0.4534(11) 0.6348(9) 0.7134(10) 0.042(2) Uani 1 1 d . . . C22 C 0.5459(15) 0.5650(12) 0.7104(12) 0.055(3) Uani 1 1 d . . . H22A H 0.6248 0.5785 0.6686 0.067 Uiso 1 1 calc R . . C23 C 0.519(3) 0.475(2) 0.770(2) 0.077(6) Uani 1 1 d . . . H23A H 0.5846 0.4302 0.7716 0.092 Uiso 1 1 calc R . . C24 C 0.404(2) 0.4486(12) 0.8274(14) 0.070(4) Uani 1 1 d . . . H24A H 0.3876 0.3840 0.8642 0.083 Uiso 1 1 calc R . . C25 C 0.310(2) 0.5166(15) 0.8313(16) 0.076(4) Uani 1 1 d . . . H25A H 0.2292 0.4994 0.8709 0.091 Uiso 1 1 calc R . . C26 C 0.337(2) 0.6134(18) 0.7744(17) 0.068(4) Uani 1 1 d . . . H26A H 0.2756 0.6625 0.7781 0.081 Uiso 1 1 calc R . . C27 C 0.5246(12) 0.3160(9) 0.2811(10) 0.044(2) Uani 1 1 d . . . C28 C 0.6413(18) 0.3357(16) 0.2172(16) 0.071(4) Uani 1 1 d . . . H28A H 0.7053 0.2893 0.2151 0.085 Uiso 1 1 calc R . . C29 C 0.659(2) 0.427(2) 0.157(2) 0.088(6) Uani 1 1 d . . . H29A H 0.7400 0.4460 0.1180 0.106 Uiso 1 1 calc R . . C30 C 0.559(3) 0.4905(19) 0.1520(18) 0.086(5) Uani 1 1 d . . . H30A H 0.5689 0.5478 0.1069 0.103 Uiso 1 1 calc R . . C31 C 0.446(2) 0.4675(17) 0.2146(17) 0.078(5) Uani 1 1 d . . . H31A H 0.3805 0.5120 0.2130 0.094 Uiso 1 1 calc R . . C32 C 0.4246(14) 0.3834(12) 0.2794(12) 0.055(3) Uani 1 1 d . . . H32A H 0.3461 0.3704 0.3216 0.065 Uiso 1 1 calc R . . C33 C 0.6441(14) 0.2717(12) 0.4945(15) 0.052(4) Uani 1 1 d . . . C34 C 0.6407(15) 0.2076(13) 0.5833(14) 0.060(3) Uani 1 1 d . . . H34A H 0.5700 0.1336 0.5776 0.071 Uiso 1 1 calc R . . C35 C 0.7413(17) 0.2548(18) 0.6764(15) 0.075(4) Uani 1 1 d . . . H35A H 0.7391 0.2115 0.7339 0.090 Uiso 1 1 calc R . . C36 C 0.8467(16) 0.3646(16) 0.6896(13) 0.067(4) Uani 1 1 d . . . H36A H 0.9137 0.3963 0.7552 0.081 Uiso 1 1 calc R . . C37 C 0.850(2) 0.4259(15) 0.6032(16) 0.069(4) Uani 1 1 d . . . H37A H 0.9219 0.4995 0.6098 0.083 Uiso 1 1 calc R . . C38 C 0.7488(12) 0.3810(12) 0.5060(12) 0.053(3) Uani 1 1 d . . . H38A H 0.7521 0.4248 0.4489 0.064 Uiso 1 1 calc R . . C39 C 0.5377(12) 0.0745(11) 0.2918(11) 0.048(2) Uani 1 1 d . . . C40 C 0.6334(14) 0.0223(13) 0.3357(17) 0.066(4) Uani 1 1 d . . . H40A H 0.6817 0.0542 0.4095 0.080 Uiso 1 1 calc R . . C41 C 0.657(2) -0.0800(16) 0.267(2) 0.084(6) Uani 1 1 d . . . H41A H 0.7273 -0.1124 0.2922 0.101 Uiso 1 1 calc R . . C42 C 0.573(3) -0.1342(14) 0.158(2) 0.082(5) Uani 1 1 d . . . H42A H 0.5844 -0.2048 0.1144 0.099 Uiso 1 1 calc R . . C43 C 0.476(2) -0.0826(15) 0.1188(17) 0.077(5) Uani 1 1 d . . . H43A H 0.4211 -0.1179 0.0478 0.093 Uiso 1 1 calc R . . C44 C 0.4582(18) 0.027(2) 0.1862(18) 0.062(4) Uani 1 1 d . . . H44A H 0.3942 0.0642 0.1587 0.075 Uiso 1 1 calc R . . C45 C 0.3328(11) 0.1782(9) 0.4221(11) 0.045(2) Uani 1 1 d . . . C46 C 0.2150(15) 0.0836(13) 0.3641(13) 0.058(3) Uani 1 1 d . . . H46A H 0.2277 0.0288 0.3013 0.069 Uiso 1 1 calc R . . C47 C 0.0788(16) 0.0700(17) 0.3988(16) 0.071(5) Uani 1 1 d . . . H47A H -0.0004 0.0056 0.3606 0.086 Uiso 1 1 calc R . . C48 C 0.0614(15) 0.1550(15) 0.4929(13) 0.066(4) Uani 1 1 d . . . H48A H -0.0303 0.1474 0.5162 0.079 Uiso 1 1 calc R . . C49 C 0.1791(15) 0.2495(14) 0.5511(14) 0.063(3) Uani 1 1 d . . . H49A H 0.1682 0.3041 0.6148 0.076 Uiso 1 1 calc R . . C50 C 0.3150(17) 0.2615(17) 0.5120(15) 0.065(4) Uani 1 1 d . . . H50A H 0.3943 0.3272 0.5478 0.078 Uiso 1 1 calc R . . P2 P 0.5087(3) 0.2086(2) 0.3711(3) 0.0421(5) Uani 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 0.0663(3) 0.04615(19) 0.0445(2) 0.01067(14) 0.00707(17) 0.02146(16) Mo1 0.0610(6) 0.1009(10) 0.0365(7) 0.0002(6) -0.0040(5) 0.0431(6) Cl1 0.109(3) 0.085(3) 0.0388(19) 0.0238(18) 0.0158(19) 0.050(2) Cl2 0.118(4) 0.081(3) 0.052(2) 0.0118(18) 0.010(2) 0.062(3) Cl3 0.116(4) 0.094(3) 0.050(2) 0.009(2) 0.022(2) 0.065(3) Cl4 0.116(4) 0.053(2) 0.093(4) 0.021(2) -0.002(3) -0.009(2) Cl5 0.094(3) 0.092(3) 0.057(2) 0.0189(18) 0.0209(18) 0.055(2) Cl6 0.136(4) 0.102(3) 0.064(3) 0.018(2) 0.019(3) 0.071(3) C1 0.046(5) 0.041(5) 0.052(6) 0.014(4) 0.008(5) 0.026(4) C2 0.045(6) 0.065(7) 0.044(6) 0.004(5) -0.008(5) 0.020(5) O1 0.053(5) 0.045(5) 0.082(8) 0.009(5) -0.002(5) 0.027(4) O2 0.062(5) 0.020(3) 0.070(7) 0.012(3) 0.010(4) 0.018(3) O3 0.050(5) 0.062(5) 0.082(7) 0.019(5) 0.001(4) 0.030(4) O4 0.044(4) 0.069(6) 0.075(7) 0.022(5) -0.014(4) 0.020(4) O5 0.069(6) 0.025(3) 0.111(9) 0.016(4) -0.006(5) -0.011(3) P1 0.0338(11) 0.0425(11) 0.0442(14) 0.0121(10) 0.0055(9) 0.0102(9) C3 0.036(4) 0.041(4) 0.061(7) 0.018(4) 0.010(4) 0.013(4) C4 0.052(6) 0.062(7) 0.075(9) 0.024(6) 0.005(6) 0.025(5) C5 0.077(10) 0.067(9) 0.115(16) 0.028(10) 0.033(10) 0.044(8) C6 0.080(10) 0.049(7) 0.098(13) 0.014(8) 0.034(9) 0.022(7) C7 0.074(9) 0.069(8) 0.059(9) 0.002(6) 0.017(7) 0.024(7) C8 0.075(8) 0.068(7) 0.048(7) 0.014(6) 0.014(6) 0.034(6) C9 0.028(4) 0.059(6) 0.042(5) 0.012(4) 0.002(4) 0.013(4) C10 0.050(6) 0.043(5) 0.065(8) 0.015(5) 0.011(5) -0.001(4) C11 0.042(6) 0.067(8) 0.075(10) 0.007(7) 0.000(6) 0.002(5) C12 0.054(8) 0.076(9) 0.071(11) 0.008(8) -0.006(7) 0.014(7) C13 0.070(9) 0.103(12) 0.040(7) 0.018(7) -0.009(6) 0.034(8) C14 0.049(6) 0.047(6) 0.057(8) 0.023(6) 0.000(5) 0.001(5) C15 0.038(5) 0.043(6) 0.036(5) 0.007(4) 0.007(4) 0.008(4) C16 0.047(6) 0.051(5) 0.052(7) -0.002(5) 0.012(5) 0.012(4) C17 0.059(7) 0.068(8) 0.067(9) 0.013(6) 0.020(6) 0.023(6) C18 0.043(6) 0.074(8) 0.072(9) 0.023(7) 0.023(6) 0.019(5) C19 0.033(5) 0.077(8) 0.066(9) 0.006(7) 0.008(5) -0.002(5) C20 0.041(6) 0.064(7) 0.050(7) 0.007(6) 0.008(5) 0.006(5) C21 0.039(5) 0.045(5) 0.047(5) 0.016(4) 0.009(4) 0.015(4) C22 0.053(6) 0.059(6) 0.055(7) 0.003(5) 0.002(5) 0.025(5) C23 0.096(13) 0.068(10) 0.084(14) 0.035(10) 0.008(10) 0.041(9) C24 0.104(12) 0.046(6) 0.064(9) 0.020(6) 0.007(8) 0.027(7) C25 0.088(11) 0.071(8) 0.082(11) 0.042(8) 0.043(9) 0.022(8) C26 0.082(10) 0.080(11) 0.068(10) 0.032(9) 0.036(8) 0.052(9) C27 0.047(5) 0.039(4) 0.046(5) 0.013(4) 0.006(4) 0.010(4) C28 0.072(9) 0.084(9) 0.082(11) 0.044(9) 0.035(8) 0.042(8) C29 0.075(10) 0.110(14) 0.098(15) 0.066(13) 0.031(10) 0.023(10) C30 0.125(17) 0.079(11) 0.074(11) 0.036(9) 0.044(11) 0.041(11) C31 0.102(13) 0.074(9) 0.076(11) 0.022(8) 0.012(9) 0.048(9) C32 0.048(6) 0.066(7) 0.052(7) 0.017(6) 0.009(5) 0.019(5) C33 0.037(5) 0.033(5) 0.080(10) 0.015(6) -0.004(5) 0.000(4) C34 0.054(7) 0.060(7) 0.068(9) 0.026(6) 0.007(6) 0.014(5) C35 0.068(9) 0.103(12) 0.070(10) 0.039(9) 0.014(8) 0.035(9) C36 0.056(7) 0.096(10) 0.048(7) -0.005(7) -0.009(6) 0.037(7) C37 0.056(8) 0.060(8) 0.068(10) -0.011(7) -0.006(7) 0.002(7) C38 0.036(5) 0.059(6) 0.059(7) 0.016(5) -0.003(5) 0.006(4) C39 0.040(5) 0.054(5) 0.056(7) 0.017(5) 0.019(5) 0.016(4) C40 0.043(6) 0.061(7) 0.097(12) 0.022(7) 0.008(6) 0.016(5) C41 0.066(9) 0.061(8) 0.134(19) 0.018(10) 0.018(10) 0.033(7) C42 0.106(14) 0.046(7) 0.101(14) 0.016(8) 0.044(11) 0.029(8) C43 0.080(10) 0.068(8) 0.075(11) 0.000(8) 0.031(8) 0.012(8) C44 0.046(7) 0.080(11) 0.065(10) 0.023(8) 0.013(6) 0.019(7) C45 0.039(5) 0.034(4) 0.060(7) 0.018(5) 0.008(4) 0.005(4) C46 0.046(6) 0.057(6) 0.060(8) 0.008(6) 0.009(5) 0.000(5) C47 0.042(7) 0.074(10) 0.075(10) 0.005(8) 0.009(6) -0.011(6) C48 0.044(6) 0.080(9) 0.063(8) 0.010(7) 0.017(5) 0.005(6) C49 0.057(7) 0.071(8) 0.063(8) 0.016(6) 0.024(6) 0.016(6) C50 0.051(7) 0.070(9) 0.058(9) -0.003(7) -0.005(6) 0.006(6) P2 0.0323(11) 0.0443(12) 0.0486(14) 0.0122(11) 0.0049(9) 0.0084(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Re1 O2 2.096(10) . ? Re1 O1 2.099(12) . ? Re1 Cl2 2.258(5) . ? Re1 Cl4 2.263(5) . ? Re1 Cl3 2.331(6) . ? Re1 Cl1 2.343(5) . ? Mo1 O5 1.778(8) . ? Mo1 O6 1.812(13) . ? Mo1 O3 2.239(11) . ? Mo1 O4 2.253(10) . ? Mo1 Cl6 2.334(5) . ? Mo1 Cl5 2.382(4) . ? C1 O4 1.232(15) . ? C1 O1 1.253(15) . ? C1 C2 1.503(13) . ? C2 O3 1.238(16) . ? C2 O2 1.246(16) . ? P1 C3 1.791(12) . ? P1 C9 1.794(11) . ? P1 C21 1.794(11) . ? P1 C15 1.817(13) . ? C3 C8 1.392(19) . ? C3 C4 1.426(16) . ? C4 C5 1.35(2) . ? C5 C6 1.35(3) . ? C6 C7 1.41(3) . ? C7 C8 1.37(2) . ? C9 C14 1.403(19) . ? C9 C10 1.406(15) . ? C10 C11 1.41(2) . ? C11 C12 1.32(3) . ? C12 C13 1.38(3) . ? C13 C14 1.40(2) . ? C15 C20 1.355(18) . ? C15 C16 1.409(17) . ? C16 C17 1.391(18) . ? C17 C18 1.35(2) . ? C18 C19 1.35(2) . ? C19 C20 1.418(18) . ? C21 C22 1.368(17) . ? C21 C26 1.37(2) . ? C22 C23 1.36(3) . ? C23 C24 1.34(3) . ? C24 C25 1.36(2) . ? C25 C26 1.41(2) . ? C27 C28 1.392(19) . ? C27 C32 1.411(18) . ? C27 P2 1.792(11) . ? C28 C29 1.39(2) . ? C29 C30 1.38(3) . ? C30 C31 1.35(3) . ? C31 C32 1.35(2) . ? C33 C38 1.370(16) . ? C33 C34 1.41(2) . ? C33 P2 1.801(15) . ? C34 C35 1.35(2) . ? C35 C36 1.37(3) . ? C36 C37 1.37(3) . ? C37 C38 1.39(2) . ? C39 C44 1.37(2) . ? C39 C40 1.373(19) . ? C39 P2 1.779(12) . ? C40 C41 1.40(2) . ? C41 C42 1.42(3) . ? C42 C43 1.35(3) . ? C43 C44 1.44(3) . ? C45 C50 1.36(2) . ? C45 C46 1.381(16) . ? C45 P2 1.803(11) . ? C46 C47 1.38(2) . ? C47 C48 1.41(2) . ? C48 C49 1.38(2) . ? C49 C50 1.40(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Re1 O1 80.1(4) . . ? O2 Re1 Cl2 172.3(3) . . ? O1 Re1 Cl2 92.3(3) . . ? O2 Re1 Cl4 92.7(3) . . ? O1 Re1 Cl4 172.8(4) . . ? Cl2 Re1 Cl4 94.8(2) . . ? O2 Re1 Cl3 86.5(4) . . ? O1 Re1 Cl3 87.1(5) . . ? Cl2 Re1 Cl3 91.6(2) . . ? Cl4 Re1 Cl3 91.4(3) . . ? O2 Re1 Cl1 88.5(4) . . ? O1 Re1 Cl1 89.0(4) . . ? Cl2 Re1 Cl1 92.97(19) . . ? Cl4 Re1 Cl1 91.9(2) . . ? Cl3 Re1 Cl1 174.1(2) . . ? O5 Mo1 O6 105.6(5) . . ? O5 Mo1 O3 164.0(4) . . ? O6 Mo1 O3 90.4(5) . . ? O5 Mo1 O4 91.8(4) . . ? O6 Mo1 O4 162.6(5) . . ? O3 Mo1 O4 72.3(3) . . ? O5 Mo1 Cl6 97.1(5) . . ? O6 Mo1 Cl6 97.2(4) . . ? O3 Mo1 Cl6 81.6(4) . . ? O4 Mo1 Cl6 80.7(3) . . ? O5 Mo1 Cl5 95.1(5) . . ? O6 Mo1 Cl5 94.9(4) . . ? O3 Mo1 Cl5 82.3(4) . . ? O4 Mo1 Cl5 82.9(3) . . ? Cl6 Mo1 Cl5 159.85(18) . . ? O4 C1 O1 123.1(12) . . ? O4 C1 C2 118.1(9) . . ? O1 C1 C2 118.9(10) . . ? O3 C2 O2 124.4(12) . . ? O3 C2 C1 117.2(11) . . ? O2 C2 C1 118.4(11) . . ? C1 O1 Re1 111.0(9) . . ? C2 O2 Re1 111.6(9) . . ? C2 O3 Mo1 116.5(9) . . ? C1 O4 Mo1 115.8(7) . . ? C3 P1 C9 110.5(5) . . ? C3 P1 C21 109.1(5) . . ? C9 P1 C21 110.0(5) . . ? C3 P1 C15 110.4(6) . . ? C9 P1 C15 106.6(6) . . ? C21 P1 C15 110.2(6) . . ? C8 C3 C4 119.3(12) . . ? C8 C3 P1 120.0(9) . . ? C4 C3 P1 120.7(10) . . ? C5 C4 C3 118.8(15) . . ? C6 C5 C4 122.6(17) . . ? C5 C6 C7 119.3(15) . . ? C8 C7 C6 119.7(16) . . ? C7 C8 C3 119.7(15) . . ? C14 C9 C10 121.1(11) . . ? C14 C9 P1 118.7(9) . . ? C10 C9 P1 120.1(10) . . ? C11 C10 C9 118.2(13) . . ? C12 C11 C10 120.1(13) . . ? C11 C12 C13 123.3(16) . . ? C12 C13 C14 119.2(15) . . ? C9 C14 C13 118.0(14) . . ? C20 C15 C16 121.9(12) . . ? C20 C15 P1 121.8(10) . . ? C16 C15 P1 115.9(9) . . ? C17 C16 C15 117.4(12) . . ? C18 C17 C16 121.7(14) . . ? C17 C18 C19 120.0(12) . . ? C18 C19 C20 121.5(12) . . ? C15 C20 C19 117.4(13) . . ? C22 C21 C26 120.4(12) . . ? C22 C21 P1 121.2(10) . . ? C26 C21 P1 118.1(10) . . ? C23 C22 C21 118.2(15) . . ? C24 C23 C22 123.2(18) . . ? C23 C24 C25 119.6(14) . . ? C24 C25 C26 118.9(15) . . ? C21 C26 C25 119.6(14) . . ? C28 C27 C32 120.5(11) . . ? C28 C27 P2 118.8(10) . . ? C32 C27 P2 120.6(9) . . ? C29 C28 C27 117.6(15) . . ? C30 C29 C28 121.8(17) . . ? C31 C30 C29 118.4(17) . . ? C32 C31 C30 123.4(17) . . ? C31 C32 C27 118.0(13) . . ? C38 C33 C34 118.9(13) . . ? C38 C33 P2 122.0(12) . . ? C34 C33 P2 119.1(9) . . ? C35 C34 C33 119.4(13) . . ? C34 C35 C36 122.5(15) . . ? C37 C36 C35 118.0(14) . . ? C36 C37 C38 121.6(15) . . ? C33 C38 C37 119.7(15) . . ? C44 C39 C40 122.8(15) . . ? C44 C39 P2 115.9(12) . . ? C40 C39 P2 121.4(11) . . ? C39 C40 C41 118.6(17) . . ? C40 C41 C42 120.1(17) . . ? C43 C42 C41 119.6(16) . . ? C42 C43 C44 120.5(19) . . ? C39 C44 C43 118.2(18) . . ? C50 C45 C46 120.4(13) . . ? C50 C45 P2 117.3(9) . . ? C46 C45 P2 121.8(11) . . ? C47 C46 C45 120.4(14) . . ? C46 C47 C48 118.9(13) . . ? C49 C48 C47 120.7(13) . . ? C48 C49 C50 118.6(14) . . ? C45 C50 C49 120.8(14) . . ? C39 P2 C27 108.6(6) . . ? C39 P2 C33 109.2(7) . . ? C27 P2 C33 109.7(6) . . ? C39 P2 C45 112.0(5) . . ? C27 P2 C45 109.8(5) . . ? C33 P2 C45 107.4(7) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 31.25 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 8.309 _refine_diff_density_min -1.439 _refine_diff_density_rms 0.251