Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof Marcetta Darensbourg' _publ_contact_author_address ; Department of Chemistry Texas A & M University College Station TX 77843-3225 USA ; _publ_contact_author_email MARCETTA@MAIL.CHEM.TAMU.EDU _publ_section_title ; Metallodithiolato Ligands as Bridges in Multiply Bonded Dimolybdenum Complexes ; loop_ _publ_author_name 'Marcetta Darensbourg' 'Stephen P. Jeffery' 'Jonghyuk Lee' data_md _database_code_depnum_ccdc_archive 'CCDC 254616' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H84 B4 F16 Mo2 N12 Ni4 S8' _chemical_formula_weight 1811.67 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.693(4) _cell_length_b 20.039(5) _cell_length_c 14.166(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.659(4) _cell_angle_gamma 90.00 _cell_volume 3393.3(16) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 1011 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 23.28 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.773 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 1.779 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7009 _exptl_absorpt_correction_T_max 0.9550 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 14270 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 23.28 _reflns_number_total 4870 _reflns_number_gt 4422 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.1135P)^2^+7.6733P] 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 4870 _refine_ls_number_parameters 406 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0621 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1569 _refine_ls_wR_factor_gt 0.1524 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.041 _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 Mo1 Mo 0.58502(4) 1.01115(2) 0.54636(3) 0.0232(2) Uani 1 1 d . . . S1 S 0.60381(11) 0.93637(6) 0.69355(9) 0.0259(3) Uani 1 1 d . . . Ni1 Ni 0.51014(5) 0.84727(3) 0.63552(5) 0.0244(2) Uani 1 1 d . . . N1 N 0.6364(4) 0.7916(2) 0.7020(3) 0.0313(10) Uani 1 1 d . . . C1 C 0.7428(4) 0.8968(3) 0.7422(4) 0.0307(12) Uani 1 1 d . . . H1A H 0.7751 0.8915 0.6881 0.037 Uiso 1 1 calc R . . H1B H 0.7943 0.9243 0.7963 0.037 Uiso 1 1 calc R . . Ni2 Ni 0.59939(6) 0.91512(4) 0.32682(5) 0.0297(2) Uani 1 1 d . . . S2 S 0.68713(11) 0.92404(7) 0.48378(10) 0.0313(3) Uani 1 1 d . . . N2 N 0.4383(4) 0.7630(2) 0.5897(3) 0.0274(10) Uani 1 1 d . . . C2 C 0.7243(5) 0.8297(3) 0.7820(4) 0.0351(13) Uani 1 1 d . . . H2A H 0.7952 0.8042 0.8036 0.042 Uiso 1 1 calc R . . H2B H 0.7001 0.8359 0.8410 0.042 Uiso 1 1 calc R . . S3 S 0.63921(11) 1.09750(6) 0.44042(10) 0.0262(3) Uani 1 1 d . . . N3 N 0.7333(4) 0.9305(3) 0.2953(4) 0.0413(12) Uani 1 1 d . . . C3 C 0.5921(4) 0.7351(3) 0.7465(4) 0.0306(12) Uani 1 1 d . . . H3A H 0.5917 0.7478 0.8139 0.037 Uiso 1 1 calc R . . H3B H 0.6410 0.6956 0.7537 0.037 Uiso 1 1 calc R . . N4 N 0.5326(4) 0.9039(3) 0.1847(4) 0.0495(14) Uani 1 1 d . . . S4 S 0.55571(11) 1.10620(6) 0.65078(10) 0.0287(3) Uani 1 1 d . . . C4 C 0.4729(5) 0.7180(3) 0.6787(4) 0.0318(12) Uani 1 1 d . . . H4A H 0.4699 0.6710 0.6563 0.038 Uiso 1 1 calc R . . H4B H 0.4206 0.7231 0.7167 0.038 Uiso 1 1 calc R . . N5 N 0.3105(5) 0.5771(3) 0.5003(4) 0.0556(15) Uani 1 1 d . . . C5 C 0.6805(4) 0.7670(3) 0.6233(4) 0.0319(12) Uani 1 1 d . . . H5A H 0.7544 0.7459 0.6559 0.038 Uiso 1 1 calc R . . H5B H 0.6913 0.8055 0.5836 0.038 Uiso 1 1 calc R . . C6 C 0.6036(5) 0.7173(3) 0.5539(4) 0.0373(14) Uani 1 1 d . . . H6A H 0.6078 0.6749 0.5909 0.045 Uiso 1 1 calc R . . H6B H 0.6315 0.7084 0.4978 0.045 Uiso 1 1 calc R . . N6 N 0.4901(6) 0.7006(4) 0.2804(5) 0.0675(17) Uani 1 1 d . . . C7 C 0.4814(5) 0.7381(3) 0.5104(4) 0.0319(12) Uani 1 1 d . . . H7A H 0.4736 0.7736 0.4599 0.038 Uiso 1 1 calc R . . H7B H 0.4361 0.6994 0.4762 0.038 Uiso 1 1 calc R . . C8 C 0.3136(4) 0.7710(3) 0.5496(4) 0.0305(12) Uani 1 1 d . . . H8A H 0.2845 0.7751 0.6061 0.037 Uiso 1 1 calc R . . H8B H 0.2792 0.7311 0.5100 0.037 Uiso 1 1 calc R . . C9 C 0.8183(5) 0.9569(5) 0.4719(5) 0.058(2) Uani 1 1 d . . . H9A H 0.8123 1.0057 0.4606 0.070 Uiso 1 1 calc R . . H9B H 0.8819 0.9480 0.5340 0.070 Uiso 1 1 calc R . . C10 C 0.8361(6) 0.9233(4) 0.3863(6) 0.060(2) Uani 1 1 d . . . H10A H 0.8521 0.8754 0.4018 0.072 Uiso 1 1 calc R . . H10B H 0.9011 0.9434 0.3732 0.072 Uiso 1 1 calc R . . C11 C 0.7200(5) 0.9947(3) 0.2414(5) 0.0435(16) Uani 1 1 d . . . H11A H 0.7909 1.0054 0.2301 0.052 Uiso 1 1 calc R . . H11B H 0.7061 1.0302 0.2844 0.052 Uiso 1 1 calc R . . C12 C 0.6281(7) 0.9954(3) 0.1438(5) 0.058(2) Uani 1 1 d . . . H12A H 0.6141 1.0424 0.1215 0.069 Uiso 1 1 calc R . . H12B H 0.6544 0.9719 0.0944 0.069 Uiso 1 1 calc R . . C13 C 0.5238(7) 0.9666(4) 0.1400(6) 0.063(2) Uani 1 1 d . . . H13A H 0.4864 0.9972 0.1735 0.075 Uiso 1 1 calc R . . H13B H 0.4755 0.9627 0.0690 0.075 Uiso 1 1 calc R . . C14 C 0.7331(7) 0.8745(3) 0.2213(8) 0.081(3) Uani 1 1 d . . . H14A H 0.7688 0.8340 0.2585 0.097 Uiso 1 1 calc R . . H14B H 0.7764 0.8885 0.1781 0.097 Uiso 1 1 calc R . . C15 C 0.6070(8) 0.8581(3) 0.1535(5) 0.062(2) Uani 1 1 d . . . H15A H 0.5970 0.8650 0.0818 0.075 Uiso 1 1 calc R . . H15B H 0.5888 0.8112 0.1631 0.075 Uiso 1 1 calc R . . C16 C 0.4185(7) 0.8673(4) 0.1591(6) 0.0606(19) Uani 1 1 d . . . H16A H 0.3769 0.8703 0.0863 0.073 Uiso 1 1 calc R . . H16B H 0.4307 0.8196 0.1777 0.073 Uiso 1 1 calc R . . C17 C 0.7174(4) 1.1679(3) 0.5154(4) 0.0319(12) Uani 1 1 d . . . H17A H 0.6971 1.1738 0.5765 0.038 Uiso 1 1 calc R . . H17B H 0.7989 1.1596 0.5358 0.038 Uiso 1 1 calc R . . C18 C 0.6456(5) 1.1005(3) 0.7843(4) 0.0345(13) Uani 1 1 d . . . H18A H 0.6615 1.0534 0.8048 0.041 Uiso 1 1 calc R . . H18B H 0.7175 1.1240 0.7955 0.041 Uiso 1 1 calc R . . C19 C 0.3423(6) 0.5234(4) 0.5172(5) 0.0447(15) Uani 1 1 d . . . C20 C 0.3860(6) 0.4562(3) 0.5408(5) 0.0476(16) Uani 1 1 d . . . H20A H 0.4094 0.4393 0.4860 0.071 Uiso 1 1 calc R . . H20B H 0.3277 0.4271 0.5493 0.071 Uiso 1 1 calc R . . H20C H 0.4504 0.4568 0.6030 0.071 Uiso 1 1 calc R . . C21 C 0.5288(6) 0.6793(4) 0.2253(6) 0.0494(16) Uani 1 1 d . . . C22 C 0.5760(6) 0.6514(4) 0.1530(6) 0.0561(18) Uani 1 1 d . . . H22A H 0.6577 0.6552 0.1795 0.084 Uiso 1 1 calc R . . H22B H 0.5470 0.6760 0.0897 0.084 Uiso 1 1 calc R . . H22C H 0.5549 0.6043 0.1414 0.084 Uiso 1 1 calc R . . B1 B 0.5878(5) 0.5461(3) 0.7809(5) 0.0286(13) Uani 1 1 d . . . F1 F 0.5470(3) 0.59902(16) 0.8219(3) 0.0447(9) Uani 1 1 d . . . F2 F 0.5259(3) 0.48832(16) 0.7819(3) 0.0410(8) Uani 1 1 d . . . F3 F 0.6990(3) 0.53630(17) 0.8368(3) 0.0403(8) Uani 1 1 d . . . F4 F 0.5797(3) 0.56121(17) 0.6827(2) 0.0432(8) Uani 1 1 d . . . B2A B 0.8646(17) 0.7041(10) 0.3980(15) 0.042(3) Uani 0.228(8) 1 d PD A -1 F5A F 0.809(3) 0.7214(18) 0.3006(16) 0.042(3) Uani 0.228(8) 1 d PD A -1 F6A F 0.8302(13) 0.7449(8) 0.4642(11) 0.042(3) Uani 0.228(8) 1 d PD A -1 F7A F 0.8444(13) 0.6373(7) 0.4188(12) 0.042(3) Uani 0.228(8) 1 d PD A -1 F8A F 0.9778(11) 0.7157(9) 0.4205(10) 0.042(3) Uani 0.228(8) 1 d PD A -1 B2B B 0.8651(12) 0.6989(7) 0.3935(11) 0.0829(11) Uani 0.772(8) 1 d PD A -2 F5B F 0.8091(13) 0.7216(8) 0.2991(8) 0.0829(11) Uani 0.77 1 d PD A -2 F6B F 0.8831(7) 0.7499(3) 0.4634(5) 0.0829(11) Uani 0.77 1 d PD A -2 F7B F 0.7979(7) 0.6500(4) 0.4175(6) 0.0829(11) Uani 0.77 1 d PD A -2 F8B F 0.9662(6) 0.6725(4) 0.3982(5) 0.0829(11) Uani 0.77 1 d PD A -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0242(3) 0.0185(3) 0.0262(3) 0.00211(16) 0.0076(2) 0.00065(16) S1 0.0295(7) 0.0215(7) 0.0255(7) 0.0017(5) 0.0078(5) -0.0019(5) Ni1 0.0252(4) 0.0185(4) 0.0269(4) 0.0005(3) 0.0053(3) 0.0016(3) N1 0.030(2) 0.028(2) 0.034(2) 0.0003(19) 0.008(2) 0.0032(19) C1 0.025(3) 0.037(3) 0.026(3) 0.004(2) 0.002(2) -0.001(2) Ni2 0.0279(4) 0.0376(4) 0.0253(4) -0.0002(3) 0.0108(3) -0.0012(3) S2 0.0295(7) 0.0353(8) 0.0288(7) 0.0021(6) 0.0093(6) 0.0093(6) N2 0.028(2) 0.021(2) 0.028(2) -0.0027(18) 0.0028(19) -0.0002(18) C2 0.032(3) 0.032(3) 0.034(3) 0.009(2) 0.002(2) 0.002(2) S3 0.0255(7) 0.0213(7) 0.0309(7) 0.0042(5) 0.0085(6) 0.0015(5) N3 0.031(3) 0.063(3) 0.032(3) 0.010(2) 0.014(2) 0.003(2) C3 0.035(3) 0.026(3) 0.030(3) 0.009(2) 0.010(2) 0.009(2) N4 0.037(3) 0.084(4) 0.030(3) -0.003(3) 0.014(2) -0.004(3) S4 0.0320(7) 0.0234(7) 0.0336(7) -0.0008(5) 0.0149(6) -0.0018(5) C4 0.042(3) 0.024(3) 0.034(3) -0.003(2) 0.020(3) -0.007(2) N5 0.061(4) 0.063(4) 0.046(3) 0.007(3) 0.022(3) 0.004(3) C5 0.029(3) 0.027(3) 0.039(3) 0.005(2) 0.010(2) 0.002(2) C6 0.041(3) 0.035(3) 0.041(3) 0.002(3) 0.020(3) 0.005(3) N6 0.061(4) 0.072(4) 0.073(4) -0.003(4) 0.028(4) -0.001(3) C7 0.038(3) 0.023(3) 0.035(3) 0.000(2) 0.012(2) -0.002(2) C8 0.027(3) 0.024(3) 0.040(3) 0.001(2) 0.010(2) 0.000(2) C9 0.024(3) 0.097(6) 0.049(4) -0.023(4) 0.006(3) -0.001(3) C10 0.040(4) 0.087(6) 0.054(4) 0.011(4) 0.017(3) 0.005(4) C11 0.043(4) 0.037(3) 0.063(4) -0.006(3) 0.034(3) -0.008(3) C12 0.090(6) 0.038(4) 0.045(4) 0.004(3) 0.023(4) 0.023(4) C13 0.073(5) 0.066(5) 0.053(4) -0.012(4) 0.025(4) 0.015(4) C14 0.084(6) 0.034(4) 0.172(10) 0.038(5) 0.106(7) 0.031(4) C15 0.135(8) 0.024(3) 0.032(3) -0.008(3) 0.033(4) -0.009(4) C16 0.070(5) 0.054(4) 0.054(4) -0.010(3) 0.015(4) -0.008(4) C17 0.025(3) 0.029(3) 0.036(3) 0.005(2) 0.004(2) -0.004(2) C18 0.030(3) 0.037(3) 0.032(3) -0.004(2) 0.006(2) -0.006(2) C19 0.044(4) 0.057(5) 0.038(3) -0.003(3) 0.021(3) -0.004(3) C20 0.052(4) 0.044(4) 0.048(4) -0.007(3) 0.018(3) -0.004(3) C21 0.047(4) 0.046(4) 0.056(4) 0.008(3) 0.018(4) -0.003(3) C22 0.055(4) 0.050(4) 0.067(5) -0.003(3) 0.025(4) -0.003(3) B1 0.028(3) 0.027(3) 0.031(3) 0.005(3) 0.011(3) 0.000(2) F1 0.045(2) 0.0326(18) 0.062(2) -0.0034(16) 0.0259(18) 0.0029(15) F2 0.0394(19) 0.0337(18) 0.046(2) -0.0008(15) 0.0090(16) -0.0112(14) F3 0.0296(17) 0.0400(19) 0.0461(19) 0.0024(15) 0.0058(15) 0.0038(14) F4 0.046(2) 0.046(2) 0.0338(18) 0.0040(15) 0.0083(15) -0.0051(16) B2A 0.045(5) 0.051(6) 0.028(4) 0.022(4) 0.009(3) -0.008(3) F5A 0.045(5) 0.051(6) 0.028(4) 0.022(4) 0.009(3) -0.008(3) F6A 0.045(5) 0.051(6) 0.028(4) 0.022(4) 0.009(3) -0.008(3) F7A 0.045(5) 0.051(6) 0.028(4) 0.022(4) 0.009(3) -0.008(3) F8A 0.045(5) 0.051(6) 0.028(4) 0.022(4) 0.009(3) -0.008(3) B2B 0.088(2) 0.073(2) 0.079(3) 0.0113(18) 0.017(2) -0.0059(18) F5B 0.088(2) 0.073(2) 0.079(3) 0.0113(18) 0.017(2) -0.0059(18) F6B 0.088(2) 0.073(2) 0.079(3) 0.0113(18) 0.017(2) -0.0059(18) F7B 0.088(2) 0.073(2) 0.079(3) 0.0113(18) 0.017(2) -0.0059(18) F8B 0.088(2) 0.073(2) 0.079(3) 0.0113(18) 0.017(2) -0.0059(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 Mo1 2.1624(10) 3_676 ? Mo1 S2 2.5072(15) . ? Mo1 S1 2.5131(14) . ? Mo1 S4 2.5149(14) . ? Mo1 S3 2.5326(14) . ? S1 C1 1.843(5) . ? S1 Ni1 2.1494(15) . ? Ni1 N1 1.919(4) . ? Ni1 N2 1.925(4) . ? Ni1 S3 2.1457(15) 3_676 ? N1 C5 1.490(7) . ? N1 C3 1.494(7) . ? N1 C2 1.504(7) . ? C1 C2 1.507(8) . ? Ni2 N4 1.917(5) . ? Ni2 N3 1.922(5) . ? Ni2 S2 2.1330(16) . ? Ni2 S4 2.1399(16) 3_676 ? S2 C9 1.850(7) . ? N2 C4 1.491(7) . ? N2 C7 1.492(7) . ? N2 C8 1.499(7) . ? S3 C17 1.842(6) . ? S3 Ni1 2.1457(15) 3_676 ? N3 C11 1.475(8) . ? N3 C10 1.501(9) . ? N3 C14 1.537(11) . ? C3 C4 1.534(8) . ? N4 C13 1.393(10) . ? N4 C15 1.487(10) . ? N4 C16 1.554(9) . ? S4 C18 1.855(6) . ? S4 Ni2 2.1399(16) 3_676 ? N5 C19 1.145(9) . ? C5 C6 1.505(8) . ? C6 C7 1.521(8) . ? N6 C21 1.136(9) . ? C8 C17 1.503(7) 3_676 ? C9 C10 1.469(10) . ? C11 C12 1.479(10) . ? C12 C13 1.429(12) . ? C14 C15 1.599(12) . ? C16 C18 1.470(10) 3_676 ? C17 C8 1.503(7) 3_676 ? C18 C16 1.470(10) 3_676 ? C19 C20 1.453(10) . ? C21 C22 1.460(11) . ? B1 F3 1.381(7) . ? B1 F1 1.391(7) . ? B1 F4 1.394(7) . ? B1 F2 1.402(7) . ? B2A F5A 1.366(17) . ? B2A F8A 1.383(19) . ? B2A F7A 1.411(18) . ? B2A F6A 1.420(19) . ? B2B F8B 1.368(14) . ? B2B F5B 1.365(13) . ? B2B F6B 1.388(14) . ? B2B F7B 1.414(14) . ? 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 Mo1 Mo1 S2 99.81(4) 3_676 . ? Mo1 Mo1 S1 100.22(4) 3_676 . ? S2 Mo1 S1 87.83(5) . . ? Mo1 Mo1 S4 101.47(4) 3_676 . ? S2 Mo1 S4 158.70(5) . . ? S1 Mo1 S4 87.43(5) . . ? Mo1 Mo1 S3 101.29(4) 3_676 . ? S2 Mo1 S3 89.45(5) . . ? S1 Mo1 S3 158.46(5) . . ? S4 Mo1 S3 87.39(5) . . ? C1 S1 Ni1 97.05(18) . . ? C1 S1 Mo1 112.23(18) . . ? Ni1 S1 Mo1 106.99(6) . . ? N1 Ni1 N2 83.01(18) . . ? N1 Ni1 S3 175.40(14) . 3_676 ? N2 Ni1 S3 92.57(13) . 3_676 ? N1 Ni1 S1 91.84(14) . . ? N2 Ni1 S1 174.85(14) . . ? S3 Ni1 S1 92.58(6) 3_676 . ? C5 N1 C3 110.8(4) . . ? C5 N1 C2 111.2(4) . . ? C3 N1 C2 110.9(4) . . ? C5 N1 Ni1 106.7(3) . . ? C3 N1 Ni1 106.1(3) . . ? C2 N1 Ni1 111.1(3) . . ? C2 C1 S1 105.9(4) . . ? N4 Ni2 N3 83.6(2) . . ? N4 Ni2 S2 174.89(17) . . ? N3 Ni2 S2 92.07(16) . . ? N4 Ni2 S4 91.63(16) . 3_676 ? N3 Ni2 S4 174.93(17) . 3_676 ? S2 Ni2 S4 92.63(6) . 3_676 ? C9 S2 Ni2 96.0(2) . . ? C9 S2 Mo1 111.9(3) . . ? Ni2 S2 Mo1 106.04(6) . . ? C4 N2 C7 110.8(4) . . ? C4 N2 C8 111.0(4) . . ? C7 N2 C8 111.1(4) . . ? C4 N2 Ni1 105.9(3) . . ? C7 N2 Ni1 107.2(3) . . ? C8 N2 Ni1 110.7(3) . . ? N1 C2 C1 110.0(4) . . ? C17 S3 Ni1 96.18(18) . 3_676 ? C17 S3 Mo1 112.49(18) . . ? Ni1 S3 Mo1 106.21(6) 3_676 . ? C11 N3 C10 116.4(5) . . ? C11 N3 C14 108.1(5) . . ? C10 N3 C14 108.5(6) . . ? C11 N3 Ni2 107.7(4) . . ? C10 N3 Ni2 111.5(4) . . ? C14 N3 Ni2 104.0(4) . . ? N1 C3 C4 109.7(4) . . ? C13 N4 C15 112.5(5) . . ? C13 N4 C16 113.2(6) . . ? C15 N4 C16 105.9(6) . . ? C13 N4 Ni2 108.1(5) . . ? C15 N4 Ni2 106.5(4) . . ? C16 N4 Ni2 110.4(4) . . ? C18 S4 Ni2 96.78(19) . 3_676 ? C18 S4 Mo1 113.04(19) . . ? Ni2 S4 Mo1 105.16(6) 3_676 . ? N2 C4 C3 110.0(4) . . ? N1 C5 C6 112.5(4) . . ? C5 C6 C7 115.7(5) . . ? N2 C7 C6 111.6(4) . . ? N2 C8 C17 110.1(4) . 3_676 ? C10 C9 S2 107.7(5) . . ? C9 C10 N3 109.5(6) . . ? N3 C11 C12 114.2(5) . . ? C13 C12 C11 117.3(7) . . ? N4 C13 C12 114.6(6) . . ? N3 C14 C15 109.3(5) . . ? N4 C15 C14 107.6(5) . . ? C18 C16 N4 108.0(5) 3_676 . ? C8 C17 S3 106.9(4) 3_676 . ? C16 C18 S4 105.4(4) 3_676 . ? N5 C19 C20 178.2(8) . . ? N6 C21 C22 178.7(8) . . ? F3 B1 F1 108.7(5) . . ? F3 B1 F4 108.7(5) . . ? F1 B1 F4 109.8(5) . . ? F3 B1 F2 110.2(5) . . ? F1 B1 F2 109.7(5) . . ? F4 B1 F2 109.7(5) . . ? F5A B2A F8A 109.3(19) . . ? F5A B2A F7A 112.5(19) . . ? F8A B2A F7A 111.1(16) . . ? F5A B2A F6A 111(2) . . ? F8A B2A F6A 106.1(16) . . ? F7A B2A F6A 106.9(15) . . ? F8B B2B F5B 110.3(12) . . ? F8B B2B F6B 108.9(11) . . ? F5B B2B F6B 111.1(12) . . ? F8B B2B F7B 110.6(11) . . ? F5B B2B F7B 108.0(12) . . ? F6B B2B F7B 107.9(10) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.095 _refine_diff_density_min -0.736 _refine_diff_density_rms 0.152 data_mdm _database_code_depnum_ccdc_archive 'CCDC 254617' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H98 B4 F16 Mo2 N14 Ni4 S8' _chemical_formula_weight 1949.88 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.319(5) _cell_length_b 23.770(10) _cell_length_c 13.822(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.057(8) _cell_angle_gamma 90.00 _cell_volume 3698(3) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 885 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 22.78 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 1.640 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 17429 _diffrn_reflns_av_R_equivalents 0.1415 _diffrn_reflns_av_sigmaI/netI 0.2050 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6378 _reflns_number_gt 3853 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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^)+(0.1076P)^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 6378 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1456 _refine_ls_R_factor_gt 0.0865 _refine_ls_wR_factor_ref 0.2676 _refine_ls_wR_factor_gt 0.2105 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.021 _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 Mo1 Mo 0.43057(7) 1.01021(4) 0.94401(7) 0.0217(3) Uani 1 1 d . . . Ni1 Ni 0.39377(12) 0.85004(6) 1.00894(11) 0.0235(4) Uani 1 1 d . . . N1 N 0.3031(8) 0.8090(4) 0.9022(8) 0.031(2) Uani 1 1 d . . . S1 S 0.2985(2) 0.92703(11) 0.9661(2) 0.0232(6) Uani 1 1 d . . . C1 C 0.2360(9) 0.9034(4) 0.8481(8) 0.024(2) Uani 1 1 d . . . H1A H 0.1656 0.9263 0.8248 0.029 Uiso 1 1 calc R . . H1B H 0.2952 0.9066 0.8005 0.029 Uiso 1 1 calc R . . Ni2 Ni 0.69315(11) 0.95595(6) 0.80651(11) 0.0225(4) Uani 1 1 d . . . N2 N 0.4907(7) 0.7824(4) 1.0436(8) 0.028(2) Uani 1 1 d . . . S2 S 0.5017(2) 0.96096(12) 0.7981(2) 0.0235(6) Uani 1 1 d . . . C2 C 0.2010(9) 0.8425(5) 0.8599(9) 0.028(3) Uani 1 1 d . . . H2A H 0.1364 0.8403 0.9028 0.033 Uiso 1 1 calc R . . H2B H 0.1709 0.8268 0.7957 0.033 Uiso 1 1 calc R . . N3 N 0.6880(8) 0.9855(4) 0.6716(8) 0.030(2) Uani 1 1 d . . . S3 S 0.5052(2) 1.10215(11) 0.8780(2) 0.0242(6) Uani 1 1 d . . . C3 C 0.2507(11) 0.7542(5) 0.9337(11) 0.040(3) Uani 1 1 d . . . H3A H 0.1910 0.7629 0.9789 0.047 Uiso 1 1 calc R . . H3B H 0.2086 0.7358 0.8757 0.047 Uiso 1 1 calc R . . N4 N 0.8677(7) 0.9544(4) 0.8193(7) 0.024(2) Uani 1 1 d . . . S4 S 0.3074(2) 1.06978(11) 1.0441(2) 0.0231(6) Uani 1 1 d . . . C4 C 0.3322(16) 0.7161(7) 0.9789(16) 0.090(8) Uani 1 1 d . . . H4A H 0.3752 0.6998 0.9268 0.108 Uiso 1 1 calc R . . H4B H 0.2851 0.6852 1.0034 0.108 Uiso 1 1 calc R . . C5 C 0.4218(10) 0.7307(5) 1.0575(10) 0.032(3) Uani 1 1 d . . . H5A H 0.4780 0.6989 1.0678 0.038 Uiso 1 1 calc R . . H5B H 0.3823 0.7351 1.1177 0.038 Uiso 1 1 calc R . . C6 C 0.3912(10) 0.7984(5) 0.8275(10) 0.035(3) Uani 1 1 d . . . H6A H 0.3724 0.7616 0.7961 0.042 Uiso 1 1 calc R . . H6B H 0.3790 0.8276 0.7763 0.042 Uiso 1 1 calc R . . C7 C 0.5138(13) 0.7985(11) 0.8650(12) 0.096(8) Uani 1 1 d . . . H7A H 0.5392 0.8384 0.8650 0.116 Uiso 1 1 calc R . . H7B H 0.5563 0.7794 0.8153 0.116 Uiso 1 1 calc R . . C8 C 0.5643(11) 0.7755(5) 0.9590(10) 0.038(3) Uani 1 1 d . . . H8A H 0.6424 0.7935 0.9767 0.045 Uiso 1 1 calc R . . H8B H 0.5788 0.7348 0.9503 0.045 Uiso 1 1 calc R . . C9 C 0.5715(10) 0.7909(5) 1.1378(10) 0.034(3) Uani 1 1 d . . . H9A H 0.5265 0.7828 1.1938 0.041 Uiso 1 1 calc R . . H9B H 0.6387 0.7641 1.1400 0.041 Uiso 1 1 calc R . . C10 C 0.4750(10) 1.0049(5) 0.6931(9) 0.030(3) Uani 1 1 d . . . H10A H 0.3930 0.9993 0.6619 0.036 Uiso 1 1 calc R . . H10B H 0.4849 1.0449 0.7118 0.036 Uiso 1 1 calc R . . C11 C 0.5654(9) 0.9885(5) 0.6224(8) 0.027(3) Uani 1 1 d . . . H11A H 0.5433 0.9514 0.5931 0.032 Uiso 1 1 calc R . . H11B H 0.5624 1.0165 0.5692 0.032 Uiso 1 1 calc R . . C12 C 0.7646(10) 0.9556(5) 0.6061(9) 0.030(3) Uani 1 1 d . . . H12A H 0.7138 0.9407 0.5492 0.036 Uiso 1 1 calc R . . H12B H 0.8206 0.9829 0.5819 0.036 Uiso 1 1 calc R . . C13 C 0.8338(10) 0.9081(5) 0.6558(9) 0.033(3) Uani 1 1 d . . . H13A H 0.7774 0.8814 0.6809 0.040 Uiso 1 1 calc R . . H13B H 0.8759 0.8879 0.6070 0.040 Uiso 1 1 calc R . . C14 C 0.9225(9) 0.9256(5) 0.7379(9) 0.028(3) Uani 1 1 d . . . H14A H 0.9807 0.9514 0.7126 0.033 Uiso 1 1 calc R . . H14B H 0.9663 0.8919 0.7641 0.033 Uiso 1 1 calc R . . C15 C 0.7334(9) 1.0444(4) 0.6940(9) 0.028(3) Uani 1 1 d . . . H15A H 0.6858 1.0614 0.7426 0.034 Uiso 1 1 calc R . . H15B H 0.7203 1.0673 0.6340 0.034 Uiso 1 1 calc R . . C16 C 0.8636(10) 1.0480(5) 0.7325(11) 0.037(3) Uani 1 1 d . . . H16A H 0.9116 1.0346 0.6812 0.044 Uiso 1 1 calc R . . H16B H 0.8841 1.0880 0.7454 0.044 Uiso 1 1 calc R . . C17 C 0.8983(9) 1.0151(4) 0.8230(10) 0.028(3) Uani 1 1 d . . . H17A H 0.9853 1.0186 0.8392 0.034 Uiso 1 1 calc R . . H17B H 0.8600 1.0325 0.8768 0.034 Uiso 1 1 calc R . . C18 C 0.9156(8) 0.9260(5) 0.9129(9) 0.025(3) Uani 1 1 d . . . H18A H 1.0004 0.9360 0.9284 0.030 Uiso 1 1 calc R . . H18B H 0.9106 0.8847 0.9042 0.030 Uiso 1 1 calc R . . C19 C 0.3812(9) 1.1505(5) 0.8538(9) 0.027(3) Uani 1 1 d . . . H19A H 0.3410 1.1440 0.7876 0.033 Uiso 1 1 calc R . . H19B H 0.3227 1.1444 0.9012 0.033 Uiso 1 1 calc R . . C20 C 0.1527(9) 1.0570(5) 1.0029(9) 0.025(3) Uani 1 1 d . . . H20A H 0.1273 1.0798 0.9445 0.030 Uiso 1 1 calc R . . H20B H 0.1394 1.0168 0.9868 0.030 Uiso 1 1 calc R . . N5 N 1.0732(11) 0.6344(5) -0.0819(10) 0.051(3) Uani 1 1 d . . . C21 C 1.0150(13) 0.6490(6) -0.0273(15) 0.057(4) Uani 1 1 d . . . C22 C 0.9366(15) 0.6675(7) 0.0457(17) 0.087(7) Uani 1 1 d . . . H22A H 0.8719 0.6403 0.0484 0.130 Uiso 1 1 calc R . . H22B H 0.9032 0.7045 0.0274 0.130 Uiso 1 1 calc R . . H22C H 0.9826 0.6700 0.1097 0.130 Uiso 1 1 calc R . . N6 N 0.2593(8) 0.5324(4) 0.6979(8) 0.030(2) Uani 1 1 d . . . C23 C 0.3030(9) 0.5497(5) 0.7694(11) 0.034(3) Uani 1 1 d . . . C24 C 0.3513(11) 0.5733(6) 0.8638(9) 0.040(3) Uani 1 1 d . . . H24A H 0.3822 0.5428 0.9070 0.060 Uiso 1 1 calc R . . H24B H 0.2882 0.5932 0.8932 0.060 Uiso 1 1 calc R . . H24C H 0.4156 0.5996 0.8540 0.060 Uiso 1 1 calc R . . N7 N 0.3828(17) 0.7120(6) 0.3183(13) 0.097(7) Uani 1 1 d . . . C25 C 0.3326(16) 0.7529(7) 0.3040(14) 0.063(5) Uani 1 1 d . . . C26 C 0.2768(12) 0.8089(6) 0.2928(15) 0.065(5) Uani 1 1 d . . . H26A H 0.3105 0.8295 0.2408 0.097 Uiso 1 1 calc R . . H26B H 0.2919 0.8297 0.3540 0.097 Uiso 1 1 calc R . . H26C H 0.1910 0.8045 0.2762 0.097 Uiso 1 1 calc R . . B1 B 0.6475(12) 0.5956(6) 0.0486(12) 0.034(3) Uani 1 1 d . . . F1 F 0.6385(7) 0.6260(3) -0.0342(6) 0.049(2) Uani 1 1 d . . . F2 F 0.5580(7) 0.5551(3) 0.0456(6) 0.051(2) Uani 1 1 d . . . F3 F 0.6435(7) 0.6294(3) 0.1294(6) 0.055(2) Uani 1 1 d . . . F4 F 0.7590(7) 0.5658(4) 0.0577(7) 0.059(2) Uani 1 1 d . . . B2 B 0.9819(16) 0.8141(8) 0.1325(16) 0.055(5) Uani 1 1 d . . . F5 F 0.8830(8) 0.7996(4) 0.0756(11) 0.098(4) Uani 1 1 d . . . F6 F 0.9568(10) 0.8356(5) 0.2218(10) 0.105(4) Uani 1 1 d . . . F7 F 1.0556(8) 0.7676(3) 0.1503(8) 0.065(3) Uani 1 1 d . . . F8 F 1.0461(8) 0.8543(4) 0.0897(8) 0.072(3) 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 Mo1 0.0143(5) 0.0266(6) 0.0251(6) -0.0012(4) 0.0059(4) 0.0000(4) Ni1 0.0164(7) 0.0289(8) 0.0257(9) -0.0002(6) 0.0038(6) -0.0005(6) N1 0.025(5) 0.024(5) 0.044(7) -0.003(4) 0.010(5) 0.004(4) S1 0.0139(12) 0.0292(15) 0.0270(16) 0.0007(12) 0.0046(11) -0.0013(10) C1 0.019(5) 0.032(6) 0.020(6) 0.002(5) -0.006(5) 0.003(4) Ni2 0.0141(7) 0.0300(8) 0.0244(8) -0.0018(6) 0.0060(6) -0.0002(5) N2 0.016(5) 0.028(5) 0.041(7) -0.002(4) 0.007(4) -0.006(4) S2 0.0148(13) 0.0312(16) 0.0253(16) -0.0024(12) 0.0052(11) -0.0002(11) C2 0.015(5) 0.034(7) 0.033(7) 0.001(5) -0.001(5) -0.008(4) N3 0.020(5) 0.038(6) 0.034(6) -0.006(5) 0.010(4) 0.001(4) S3 0.0161(13) 0.0283(15) 0.0290(17) 0.0009(12) 0.0061(12) -0.0015(10) C3 0.039(7) 0.031(7) 0.050(9) 0.003(6) 0.015(7) -0.014(6) N4 0.017(4) 0.041(6) 0.014(5) -0.006(4) 0.003(4) -0.003(4) S4 0.0174(13) 0.0292(15) 0.0235(16) -0.0047(12) 0.0055(12) -0.0003(11) C4 0.077(13) 0.071(12) 0.107(18) 0.034(11) -0.060(12) -0.040(10) C5 0.030(6) 0.023(6) 0.042(8) -0.005(5) 0.004(6) 0.002(5) C6 0.041(7) 0.031(7) 0.036(8) -0.003(6) 0.012(6) 0.009(5) C7 0.031(8) 0.23(3) 0.029(9) 0.008(12) 0.021(7) 0.017(11) C8 0.031(7) 0.037(7) 0.042(9) -0.006(6) -0.009(6) 0.018(5) C9 0.022(6) 0.036(7) 0.045(9) 0.004(6) 0.004(6) 0.001(5) C10 0.022(6) 0.027(6) 0.039(8) -0.005(5) -0.002(5) 0.007(5) C11 0.025(6) 0.041(7) 0.017(6) -0.006(5) 0.008(5) 0.006(5) C12 0.030(6) 0.039(7) 0.024(7) 0.000(5) 0.013(5) 0.006(5) C13 0.030(6) 0.040(7) 0.028(7) -0.004(6) 0.001(5) 0.003(5) C14 0.014(5) 0.043(7) 0.027(7) 0.005(5) 0.009(5) -0.003(5) C15 0.023(6) 0.020(6) 0.043(8) 0.000(5) 0.011(5) -0.004(4) C16 0.031(7) 0.033(7) 0.048(9) 0.003(6) 0.015(6) -0.005(5) C17 0.013(5) 0.028(6) 0.046(8) -0.003(6) 0.011(5) -0.008(4) C18 0.005(5) 0.039(7) 0.031(7) -0.007(5) 0.004(5) -0.005(4) C19 0.017(5) 0.039(7) 0.025(7) 0.001(5) -0.001(5) 0.009(5) C20 0.016(5) 0.027(6) 0.033(7) -0.002(5) 0.006(5) 0.000(4) N5 0.040(7) 0.051(8) 0.062(9) 0.001(6) 0.003(7) -0.009(6) C21 0.039(8) 0.045(9) 0.089(15) 0.002(9) 0.010(9) -0.002(7) C22 0.068(12) 0.061(11) 0.14(2) -0.018(12) 0.040(13) -0.009(9) N6 0.021(5) 0.030(5) 0.039(7) 0.003(5) -0.003(5) 0.001(4) C23 0.004(5) 0.043(8) 0.056(10) 0.009(7) 0.010(6) -0.003(5) C24 0.027(6) 0.077(10) 0.017(7) 0.004(6) 0.004(5) 0.003(6) N7 0.171(18) 0.039(8) 0.093(14) 0.027(8) 0.069(13) 0.038(10) C25 0.075(12) 0.055(11) 0.063(12) 0.001(8) 0.032(10) -0.009(9) C26 0.038(8) 0.035(8) 0.122(18) -0.004(9) 0.015(9) 0.006(6) B1 0.031(7) 0.042(9) 0.030(9) -0.002(7) 0.001(6) 0.001(6) F1 0.057(5) 0.054(5) 0.038(5) 0.006(4) 0.020(4) 0.009(4) F2 0.043(5) 0.057(5) 0.054(6) -0.001(4) 0.006(4) 0.000(4) F3 0.062(5) 0.063(5) 0.038(5) -0.014(4) 0.000(4) 0.010(4) F4 0.045(5) 0.068(6) 0.062(7) 0.001(5) -0.001(4) 0.015(4) B2 0.055(11) 0.051(11) 0.062(13) 0.005(9) 0.016(10) 0.001(9) F5 0.043(5) 0.067(6) 0.178(14) -0.022(7) -0.014(7) 0.016(5) F6 0.111(9) 0.088(8) 0.128(12) -0.036(7) 0.071(9) -0.041(6) F7 0.073(6) 0.049(5) 0.071(7) 0.006(4) -0.008(5) 0.009(4) F8 0.052(5) 0.063(6) 0.101(9) 0.032(5) 0.008(5) -0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 Mo1 2.142(2) 3_677 ? Mo1 S4 2.503(3) . ? Mo1 S1 2.517(3) . ? Mo1 S2 2.535(3) . ? Mo1 S3 2.546(3) . ? Ni1 N1 1.966(10) . ? Ni1 N2 1.977(9) . ? Ni1 S3 2.159(3) 3_677 ? Ni1 S1 2.174(3) . ? N1 C2 1.473(14) . ? N1 C3 1.514(14) . ? N1 C6 1.530(15) . ? S1 C1 1.798(11) . ? C1 C2 1.514(15) . ? Ni2 N4 1.965(8) . ? Ni2 N3 1.989(11) . ? Ni2 S4 2.155(3) 3_677 ? Ni2 S2 2.162(3) . ? N2 C5 1.478(14) . ? N2 C8 1.515(17) . ? N2 C9 1.524(16) . ? S2 C10 1.787(13) . ? N3 C11 1.481(14) . ? N3 C12 1.497(14) . ? N3 C15 1.512(14) . ? S3 C19 1.818(10) . ? S3 Ni1 2.159(3) 3_677 ? C3 C4 1.39(2) . ? N4 C17 1.483(13) . ? N4 C18 1.508(15) . ? N4 C14 1.506(14) . ? S4 C20 1.809(11) . ? S4 Ni2 2.155(3) 3_677 ? C4 C5 1.45(2) . ? C6 C7 1.430(19) . ? C7 C8 1.47(2) . ? C9 C19 1.494(16) 3_677 ? C10 C11 1.537(15) . ? C12 C13 1.499(16) . ? C13 C14 1.493(16) . ? C15 C16 1.515(16) . ? C16 C17 1.492(18) . ? C18 C20 1.519(15) 3_677 ? C19 C9 1.494(16) 3_677 ? C20 C18 1.519(15) 3_677 ? N5 C21 1.109(19) . ? C21 C22 1.48(2) . ? N6 C23 1.135(17) . ? C23 C24 1.47(2) . ? N7 C25 1.133(19) . ? C25 C26 1.47(2) . ? B1 F1 1.349(17) . ? B1 F3 1.380(17) . ? B1 F2 1.395(16) . ? B1 F4 1.441(16) . ? B2 F5 1.34(2) . ? B2 F8 1.372(19) . ? B2 F6 1.39(2) . ? B2 F7 1.39(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 Mo1 Mo1 S4 97.92(9) 3_677 . ? Mo1 Mo1 S1 97.71(9) 3_677 . ? S4 Mo1 S1 90.28(9) . . ? Mo1 Mo1 S2 101.53(9) 3_677 . ? S4 Mo1 S2 160.49(10) . . ? S1 Mo1 S2 88.63(9) . . ? Mo1 Mo1 S3 101.98(9) 3_677 . ? S4 Mo1 S3 86.42(9) . . ? S1 Mo1 S3 160.30(10) . . ? S2 Mo1 S3 88.06(10) . . ? N1 Ni1 N2 90.6(4) . . ? N1 Ni1 S3 177.6(3) . 3_677 ? N2 Ni1 S3 90.9(3) . 3_677 ? N1 Ni1 S1 90.5(3) . . ? N2 Ni1 S1 175.7(3) . . ? S3 Ni1 S1 87.92(12) 3_677 . ? C2 N1 C3 105.3(9) . . ? C2 N1 C6 111.2(10) . . ? C3 N1 C6 110.9(9) . . ? C2 N1 Ni1 110.8(7) . . ? C3 N1 Ni1 113.6(8) . . ? C6 N1 Ni1 105.2(7) . . ? C1 S1 Ni1 96.9(4) . . ? C1 S1 Mo1 108.5(4) . . ? Ni1 S1 Mo1 114.23(11) . . ? C2 C1 S1 106.4(8) . . ? N4 Ni2 N3 91.2(4) . . ? N4 Ni2 S4 90.8(3) . 3_677 ? N3 Ni2 S4 175.4(3) . 3_677 ? N4 Ni2 S2 177.1(3) . . ? N3 Ni2 S2 90.0(3) . . ? S4 Ni2 S2 87.87(11) 3_677 . ? C5 N2 C8 110.6(9) . . ? C5 N2 C9 106.0(9) . . ? C8 N2 C9 110.1(9) . . ? C5 N2 Ni1 114.9(7) . . ? C8 N2 Ni1 103.8(7) . . ? C9 N2 Ni1 111.6(7) . . ? C10 S2 Ni2 99.1(4) . . ? C10 S2 Mo1 109.6(4) . . ? Ni2 S2 Mo1 112.53(12) . . ? N1 C2 C1 110.9(8) . . ? C11 N3 C12 108.6(9) . . ? C11 N3 C15 109.4(8) . . ? C12 N3 C15 111.0(8) . . ? C11 N3 Ni2 112.4(7) . . ? C12 N3 Ni2 116.0(7) . . ? C15 N3 Ni2 99.2(7) . . ? C19 S3 Ni1 98.1(4) . 3_677 ? C19 S3 Mo1 109.3(4) . . ? Ni1 S3 Mo1 111.28(13) 3_677 . ? C4 C3 N1 115.3(11) . . ? C17 N4 C18 110.1(9) . . ? C17 N4 C14 110.8(8) . . ? C18 N4 C14 107.3(8) . . ? C17 N4 Ni2 102.3(6) . . ? C18 N4 Ni2 110.7(6) . . ? C14 N4 Ni2 115.6(7) . . ? C20 S4 Ni2 98.8(4) . 3_677 ? C20 S4 Mo1 108.0(4) . . ? Ni2 S4 Mo1 115.29(12) 3_677 . ? C3 C4 C5 124.0(16) . . ? C4 C5 N2 116.0(12) . . ? C7 C6 N1 115.6(12) . . ? C6 C7 C8 126.4(14) . . ? C7 C8 N2 116.6(10) . . ? C19 C9 N2 111.6(10) 3_677 . ? C11 C10 S2 107.6(7) . . ? N3 C11 C10 112.0(9) . . ? C13 C12 N3 112.9(10) . . ? C14 C13 C12 114.6(10) . . ? C13 C14 N4 113.4(9) . . ? N3 C15 C16 114.9(9) . . ? C17 C16 C15 115.2(9) . . ? N4 C17 C16 116.2(10) . . ? N4 C18 C20 111.8(9) . 3_677 ? C9 C19 S3 108.2(8) 3_677 . ? C18 C20 S4 105.6(8) 3_677 . ? N5 C21 C22 179.1(17) . . ? N6 C23 C24 175.9(12) . . ? N7 C25 C26 174(2) . . ? F1 B1 F3 111.6(12) . . ? F1 B1 F2 110.9(12) . . ? F3 B1 F2 109.8(11) . . ? F1 B1 F4 108.9(11) . . ? F3 B1 F4 108.6(11) . . ? F2 B1 F4 106.9(11) . . ? F5 B2 F8 111.9(16) . . ? F5 B2 F6 112.2(15) . . ? F8 B2 F6 107.1(14) . . ? F5 B2 F7 110.3(14) . . ? F8 B2 F7 107.2(13) . . ? F6 B2 F7 108.0(16) . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.561 _refine_diff_density_min -1.275 _refine_diff_density_rms 0.200