Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _audit_creation_date 2004-12-04 _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? _publ_contact_author_name 'Hideki Sugimoto' _publ_contact_author_address ; Department of Chemistry Osaka City University Sumiyoshi-ku Osaka 558+8585 JAPAN ; _publ_contact_author_email sugimoto@sci.osaka-cu.ac.jp _publ_contact_author_fax +81-6-6605-2522 _publ_requested_category 'CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; A New Series of Molybdenum-(IV), -(V), and -(VI) Dithiolate Compounds as Active Site Models of Molybdoenzymes: Preparation, Crystal Structures, Spectroscopic / Electrochemical Properties, and Reactivity in Oxygen Atom Transfer ; _publ_section_references ; ENTER OTHER REFERENCES Rigaku/MSC and Rigaku Corporation. (2004). CrystalStructure 3.6.0. Single Crystal Structure Analysis Software. Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX, USA 77381-5209. Rigaku, 3-9-12 Akishima, Tokyo 196-8666, Japan. Watkin, D.J., Prout, C.K. Carruthers, J.R. & Betteridge, P.W. (1996) CRYSTALS Issue 10, Chemical Crystallography Laboratory, Oxford, UK. ; loop_ _publ_author_name 'Hideki Sugimoto' 'Hiroyuki Miyake' 'Koji Tanaka' 'Makoto Tarumizu' 'Hiroshi Tsukube' #============================================================================== data_(Et4N)2[1] _database_code_depnum_ccdc_archive 'CCDC 253876' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C28 H44 Cl4 N2 Mo O2 S4 ' _chemical_formula_moiety 'C28 H44 Cl4 N2 Mo O2 S4 ' _chemical_formula_weight 806.66 _chemical_melting_point ? _chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d 2' _symmetry_space_group_name_Hall 'F 2 -2d' _symmetry_Int_Tables_number 43 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/4-X,1/4+Y,1/4+Z 3 1/4+X,1/4-Y,1/4+Z 4 1/2-X,-Y,1/2+Z 5 +X,1/2+Y,1/2+Z 6 1/4-X,3/4+Y,3/4+Z 7 1/4+X,3/4-Y,3/4+Z 8 1/2-X,1/2-Y,+Z 9 1/2+X,+Y,1/2+Z 10 3/4-X,1/4+Y,3/4+Z 11 3/4+X,1/4-Y,3/4+Z 12 -X,-Y,+Z 13 1/2+X,1/2+Y,+Z 14 3/4-X,3/4+Y,1/4+Z 15 3/4+X,3/4-Y,1/4+Z 16 -X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 28.139(3) _cell_length_b 21.789(3) _cell_length_c 22.697(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 13916.3(29) _cell_formula_units_Z 16 _cell_measurement_reflns_used 15170 _cell_measurement_theta_min 4.1 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 123.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6656.00 _exptl_absorpt_coefficient_mu 0.952 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.713 _exptl_absorpt_correction_T_max 0.927 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 34465 _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9923 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9923 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7813 _reflns_number_gt 7013 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0380 _refine_ls_wR_factor_ref 0.0880 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 7813 _refine_ls_number_parameters 415 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.7080\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0020 _refine_diff_density_max 1.97 _refine_diff_density_min -1.09 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 3398 Friedel Pairs' _refine_ls_abs_structure_Flack -0.00(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mo Mo -1.683 0.686 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo(1) Mo 0.504240(10) 0.211960(10) 1.02808(3) 0.01674(7) Uani 1.00 1 d . . . Cl(1) Cl 0.31270(4) 0.25846(5) 0.98197(6) 0.0321(3) Uani 1.00 1 d . . . Cl(2) Cl 0.47473(4) 0.41755(4) 0.87408(5) 0.0259(2) Uani 1.00 1 d . . . Cl(3) Cl 0.53207(4) 0.07060(6) 0.82125(6) 0.0424(3) Uani 1.00 1 d . . . Cl(4) Cl 0.69519(3) 0.19608(5) 0.96146(5) 0.0296(3) Uani 1.00 1 d . . . S(1) S 0.41888(3) 0.22213(4) 1.01017(5) 0.0191(2) Uani 1.00 1 d . . . S(2) S 0.50231(3) 0.30675(4) 0.95886(5) 0.0214(2) Uani 1.00 1 d . . . S(3) S 0.50612(3) 0.14804(5) 0.93342(5) 0.0265(3) Uani 1.00 1 d . . . S(4) S 0.58961(3) 0.21090(4) 1.00720(5) 0.0199(2) Uani 1.00 1 d . . . O(1) O 0.52277(11) 0.26093(13) 1.08407(13) 0.0262(7) Uani 1.00 1 d . . . O(2) O 0.48577(10) 0.14743(13) 1.06576(13) 0.0271(8) Uani 1.00 1 d . . . N(1) N 0.39432(13) 0.2846(2) 0.7312(2) 0.0328(10) Uani 1.00 1 d . . . N(2) N 0.64718(11) 0.3700(1) 0.8795(2) 0.0220(8) Uani 1.00 1 d . . . C(1) C 0.40628(13) 0.2850(2) 0.9644(2) 0.0173(9) Uani 1.00 1 d . . . C(2) C 0.44333(12) 0.3220(2) 0.9410(2) 0.0152(8) Uani 1.00 1 d . . . C(3) C 0.4306(1) 0.3718(2) 0.9056(2) 0.0193(9) Uani 1.00 1 d . . . C(4) C 0.3836(1) 0.3869(2) 0.8936(2) 0.0220(10) Uani 1.00 1 d . . . C(5) C 0.3475(1) 0.3517(2) 0.9177(2) 0.0250(10) Uani 1.00 1 d . . . C(6) C 0.35943(13) 0.3019(2) 0.9521(2) 0.0209(9) Uani 1.00 1 d . . . C(7) C 0.5644(1) 0.1425(2) 0.9098(2) 0.0211(9) Uani 1.00 1 d . . . C(8) C 0.60155(13) 0.1700(2) 0.9425(2) 0.0179(9) Uani 1.00 1 d . . . C(9) C 0.6483(1) 0.1639(2) 0.9213(2) 0.0224(10) Uani 1.00 1 d . . . C(10) C 0.6593(2) 0.1321(2) 0.8705(2) 0.0256(10) Uani 1.00 1 d . . . C(11) C 0.6232(2) 0.1038(2) 0.8390(2) 0.0263(10) Uani 1.00 1 d . . . C(12) C 0.5765(2) 0.1095(2) 0.8593(2) 0.0265(11) Uani 1.00 1 d . . . C(13) C 0.4195(2) 0.2257(2) 0.7454(3) 0.048(2) Uani 1.00 1 d . . . C(14) C 0.4390(3) 0.2207(3) 0.8068(3) 0.077(2) Uani 1.00 1 d . . . C(15) C 0.4262(2) 0.3389(2) 0.7437(2) 0.0347(12) Uani 1.00 1 d . . . C(16) C 0.4725(2) 0.3390(3) 0.7097(3) 0.051(2) Uani 1.00 1 d . . . C(17) C 0.3507(2) 0.2929(2) 0.7704(3) 0.046(2) Uani 1.00 1 d . . . C(18) C 0.3148(2) 0.2417(4) 0.7666(5) 0.116(4) Uani 1.00 1 d . . . C(19) C 0.3804(2) 0.2822(4) 0.6671(3) 0.086(2) Uani 1.00 1 d . . . C(20) C 0.3594(4) 0.3414(7) 0.6436(3) 0.184(5) Uani 1.00 1 d . . . C(21) C 0.6768(2) 0.3696(2) 0.8238(2) 0.0295(11) Uani 1.00 1 d . . . C(22) C 0.7077(2) 0.3124(2) 0.8158(2) 0.0353(12) Uani 1.00 1 d . . . C(23) C 0.6154(1) 0.3136(2) 0.8825(2) 0.0233(10) Uani 1.00 1 d . . . C(24) C 0.5839(2) 0.3026(2) 0.8293(2) 0.0352(13) Uani 1.00 1 d . . . C(25) C 0.6781(2) 0.3683(2) 0.9339(2) 0.0276(11) Uani 1.00 1 d . . . C(26) C 0.7099(2) 0.4235(2) 0.9424(3) 0.043(1) Uani 1.00 1 d . . . C(27) C 0.6175(2) 0.4281(2) 0.8782(2) 0.0274(11) Uani 1.00 1 d . . . C(28) C 0.5902(2) 0.4411(2) 0.9345(2) 0.0327(12) Uani 1.00 1 d . . . H(1) H 0.3765 0.4214 0.8695 0.026 Uiso 1.00 1 c R . . H(2) H 0.3151 0.3616 0.9103 0.030 Uiso 1.00 1 c R . . H(3) H 0.6913 0.1296 0.8575 0.031 Uiso 1.00 1 c R . . H(4) H 0.6299 0.0810 0.8043 0.032 Uiso 1.00 1 c R . . H(5) H 0.3976 0.1930 0.7404 0.057 Uiso 1.00 1 c R . . H(6) H 0.4450 0.2211 0.7184 0.057 Uiso 1.00 1 c R . . H(7) H 0.4706 0.2362 0.8071 0.093 Uiso 1.00 1 c R . . H(8) H 0.4391 0.1791 0.8195 0.093 Uiso 1.00 1 c R . . H(9) H 0.4199 0.2444 0.8327 0.093 Uiso 1.00 1 c R . . H(10) H 0.4093 0.3753 0.7340 0.042 Uiso 1.00 1 c R . . H(11) H 0.4334 0.3388 0.7846 0.042 Uiso 1.00 1 c R . . H(12) H 0.4961 0.3179 0.7318 0.061 Uiso 1.00 1 c R . . H(13) H 0.4826 0.3800 0.7030 0.061 Uiso 1.00 1 c R . . H(14) H 0.4679 0.3189 0.6731 0.061 Uiso 1.00 1 c R . . H(15) H 0.3611 0.2967 0.8101 0.055 Uiso 1.00 1 c R . . H(16) H 0.3350 0.3295 0.7588 0.055 Uiso 1.00 1 c R . . H(17) H 0.2924 0.2496 0.7362 0.139 Uiso 1.00 1 c R . . H(18) H 0.2986 0.2377 0.8031 0.139 Uiso 1.00 1 c R . . H(19) H 0.3314 0.2047 0.7582 0.139 Uiso 1.00 1 c R . . H(20) H 0.4078 0.2721 0.6446 0.104 Uiso 1.00 1 c R . . H(21) H 0.3569 0.2513 0.6619 0.104 Uiso 1.00 1 c R . . H(22) H 0.3259 0.3420 0.6490 0.221 Uiso 1.00 1 c R . . H(23) H 0.3666 0.3459 0.6029 0.221 Uiso 1.00 1 c R . . H(24) H 0.3734 0.3741 0.6651 0.221 Uiso 1.00 1 c R . . H(25) H 0.6558 0.3723 0.7912 0.035 Uiso 1.00 1 c R . . H(26) H 0.6970 0.4046 0.8245 0.036 Uiso 1.00 1 c R . . H(27) H 0.7379 0.3192 0.8335 0.042 Uiso 1.00 1 c R . . H(28) H 0.7118 0.3040 0.7751 0.043 Uiso 1.00 1 c R . . H(29) H 0.6927 0.2783 0.8343 0.042 Uiso 1.00 1 c R . . H(30) H 0.6351 0.2786 0.8875 0.028 Uiso 1.00 1 c R . . H(31) H 0.5953 0.3179 0.9159 0.028 Uiso 1.00 1 c R . . H(32) H 0.5544 0.3231 0.8345 0.043 Uiso 1.00 1 c R . . H(33) H 0.5784 0.2599 0.8246 0.042 Uiso 1.00 1 c R . . H(34) H 0.5994 0.3182 0.7953 0.042 Uiso 1.00 1 c R . . H(35) H 0.6577 0.3656 0.9672 0.033 Uiso 1.00 1 c R . . H(36) H 0.6975 0.3327 0.9319 0.033 Uiso 1.00 1 c R . . H(37) H 0.7396 0.4160 0.9238 0.052 Uiso 1.00 1 c R . . H(38) H 0.7149 0.4303 0.9833 0.052 Uiso 1.00 1 c R . . H(39) H 0.6955 0.4587 0.9254 0.052 Uiso 1.00 1 c R . . H(40) H 0.6380 0.4618 0.8708 0.033 Uiso 1.00 1 c R . . H(41) H 0.5952 0.4244 0.8469 0.033 Uiso 1.00 1 c R . . H(42) H 0.5598 0.4223 0.9325 0.039 Uiso 1.00 1 c R . . H(43) H 0.5864 0.4842 0.9391 0.039 Uiso 1.00 1 c R . . H(44) H 0.6072 0.4251 0.9671 0.040 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mo(1) 0.0160(2) 0.01785(13) 0.0164(1) -0.00076(11) -0.00140(13) 0.00167(12) Cl(1) 0.0140(5) 0.0393(6) 0.0429(7) -0.0058(4) 0.0006(4) 0.0043(5) Cl(2) 0.0260(5) 0.0250(5) 0.0268(5) -0.0029(4) -0.0002(4) 0.0088(4) Cl(3) 0.0327(6) 0.0554(7) 0.0393(7) -0.0167(5) 0.0077(5) -0.0261(6) Cl(4) 0.0155(4) 0.0387(5) 0.0345(6) -0.0008(4) -0.0056(4) 0.0029(4) S(1) 0.0148(4) 0.0208(4) 0.0216(5) -0.0021(3) 0.0009(3) 0.0026(3) S(2) 0.0127(4) 0.0234(4) 0.0281(5) 0.0010(3) 0.0015(4) 0.0086(4) S(3) 0.0157(5) 0.0326(5) 0.0312(6) -0.0021(4) -0.0006(4) -0.0129(4) S(4) 0.0154(5) 0.0235(4) 0.0207(5) -0.0007(3) -0.0034(3) -0.0008(4) O(1) 0.028(2) 0.032(2) 0.019(2) -0.0064(12) -0.0006(12) -0.0045(11) O(2) 0.031(2) 0.028(1) 0.022(2) -0.0034(12) -0.0032(12) 0.0113(12) N(1) 0.021(2) 0.049(2) 0.029(2) 0.006(2) 0.001(2) -0.022(2) N(2) 0.018(2) 0.024(2) 0.024(2) -0.0002(12) 0.0065(13) 0.0067(13) C(1) 0.017(2) 0.022(2) 0.013(2) 0.0014(13) -0.001(1) -0.004(1) C(2) 0.016(2) 0.016(2) 0.014(2) 0.0019(12) -0.0011(13) -0.0024(13) C(3) 0.020(2) 0.020(2) 0.018(2) -0.002(1) -0.001(1) -0.003(1) C(4) 0.026(2) 0.023(2) 0.018(2) 0.010(2) -0.006(2) -0.005(1) C(5) 0.019(2) 0.029(2) 0.027(2) 0.009(2) -0.004(2) -0.004(2) C(6) 0.015(2) 0.026(2) 0.022(2) -0.003(1) -0.002(1) -0.002(2) C(7) 0.019(2) 0.019(2) 0.025(2) 0.001(1) 0.001(2) -0.004(2) C(8) 0.015(2) 0.015(2) 0.023(2) 0.0020(13) -0.003(1) 0.002(1) C(9) 0.016(2) 0.021(2) 0.030(2) 0.004(1) -0.004(2) 0.006(2) C(10) 0.019(2) 0.024(2) 0.034(2) 0.003(1) 0.005(2) 0.006(2) C(11) 0.026(2) 0.026(2) 0.026(2) 0.001(2) 0.005(2) -0.004(2) C(12) 0.023(2) 0.026(2) 0.030(2) -0.006(2) -0.000(2) -0.002(2) C(13) 0.046(3) 0.027(2) 0.069(4) 0.003(2) 0.025(3) -0.013(2) C(14) 0.106(6) 0.067(4) 0.058(4) 0.049(4) 0.036(4) 0.027(3) C(15) 0.044(3) 0.024(2) 0.036(3) 0.001(2) 0.013(2) -0.003(2) C(16) 0.054(4) 0.046(3) 0.052(4) -0.012(3) 0.023(3) -0.013(3) C(17) 0.022(2) 0.069(3) 0.047(3) 0.002(2) 0.013(2) -0.032(3) C(18) 0.032(4) 0.156(8) 0.161(10) -0.037(4) 0.050(5) -0.105(8) C(19) 0.037(3) 0.184(8) 0.037(3) 0.054(4) -0.016(3) -0.066(4) C(20) 0.170(9) 0.36(2) 0.025(4) 0.222(11) -0.022(5) -0.031(6) C(21) 0.030(2) 0.030(2) 0.029(2) 0.000(2) 0.013(2) 0.009(2) C(22) 0.035(3) 0.036(2) 0.035(3) 0.005(2) 0.013(2) 0.000(2) C(23) 0.020(2) 0.022(2) 0.028(2) -0.001(1) 0.003(2) 0.005(2) C(24) 0.030(2) 0.044(3) 0.033(3) -0.001(2) -0.000(2) -0.006(2) C(25) 0.021(2) 0.033(2) 0.029(2) -0.003(2) -0.002(2) 0.000(2) C(26) 0.025(2) 0.045(3) 0.058(3) -0.009(2) 0.002(2) -0.008(3) C(27) 0.026(2) 0.021(2) 0.035(3) 0.003(2) 0.003(2) 0.006(2) C(28) 0.025(2) 0.029(2) 0.044(3) 0.002(2) 0.007(2) 0.001(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mo(1) S(1) 2.4462(9) ? . . Mo(1) S(2) 2.596(1) ? . . Mo(1) S(3) 2.561(1) ? . . Mo(1) S(4) 2.4486(9) ? . . Mo(1) O(1) 1.739(3) ? . . Mo(1) O(2) 1.726(3) ? . . Cl(1) C(6) 1.756(4) ? . . Cl(2) C(3) 1.746(4) ? . . Cl(3) C(12) 1.742(4) ? . . Cl(4) C(9) 1.750(4) ? . . S(1) C(1) 1.755(4) ? . . S(2) C(2) 1.741(3) ? . . S(3) C(7) 1.728(4) ? . . S(4) C(8) 1.750(4) ? . . N(1) C(13) 1.502(6) ? . . N(1) C(15) 1.510(6) ? . . N(1) C(17) 1.528(6) ? . . N(1) C(19) 1.507(7) ? . . N(2) C(21) 1.514(6) ? . . N(2) C(23) 1.520(5) ? . . N(2) C(25) 1.510(6) ? . . N(2) C(27) 1.517(5) ? . . C(1) C(2) 1.421(5) ? . . C(1) C(6) 1.397(5) ? . . C(2) C(3) 1.397(5) ? . . C(3) C(4) 1.388(6) ? . . C(4) C(5) 1.386(6) ? . . C(5) C(6) 1.380(6) ? . . C(7) C(8) 1.417(5) ? . . C(7) C(12) 1.394(6) ? . . C(8) C(9) 1.407(5) ? . . C(9) C(10) 1.380(6) ? . . C(10) C(11) 1.386(6) ? . . C(11) C(12) 1.398(6) ? . . C(13) C(14) 1.502(9) ? . . C(15) C(16) 1.515(8) ? . . C(17) C(18) 1.51(1) ? . . C(19) C(20) 1.52(2) ? . . C(21) C(22) 1.531(6) ? . . C(23) C(24) 1.517(6) ? . . C(25) C(26) 1.512(7) ? . . C(27) C(28) 1.518(7) ? . . C(4) H(1) 0.9500 ? . . C(5) H(2) 0.9501 ? . . C(10) H(3) 0.9500 ? . . C(11) H(4) 0.9500 ? . . C(13) H(5) 0.9500 ? . . C(13) H(6) 0.9500 ? . . C(14) H(7) 0.9501 ? . . C(14) H(8) 0.9501 ? . . C(14) H(9) 0.9500 ? . . C(15) H(10) 0.9500 ? . . C(15) H(11) 0.9500 ? . . C(16) H(12) 0.9501 ? . . C(16) H(13) 0.9501 ? . . C(16) H(14) 0.9499 ? . . C(17) H(15) 0.9500 ? . . C(17) H(16) 0.9500 ? . . C(18) H(17) 0.9500 ? . . C(18) H(18) 0.9501 ? . . C(18) H(19) 0.9500 ? . . C(19) H(20) 0.9498 ? . . C(19) H(21) 0.9499 ? . . C(20) H(22) 0.9501 ? . . C(20) H(23) 0.9501 ? . . C(20) H(24) 0.9501 ? . . C(21) H(25) 0.9502 ? . . C(21) H(26) 0.9501 ? . . C(22) H(27) 0.9500 ? . . C(22) H(28) 0.9499 ? . . C(22) H(29) 0.9500 ? . . C(23) H(30) 0.9500 ? . . C(23) H(31) 0.9499 ? . . C(24) H(32) 0.9500 ? . . C(24) H(33) 0.9499 ? . . C(24) H(34) 0.9501 ? . . C(25) H(35) 0.9499 ? . . C(25) H(36) 0.9499 ? . . C(26) H(37) 0.9500 ? . . C(26) H(38) 0.9499 ? . . C(26) H(39) 0.9499 ? . . C(27) H(40) 0.9501 ? . . C(27) H(41) 0.9500 ? . . C(28) H(42) 0.9501 ? . . C(28) H(43) 0.9500 ? . . C(28) H(44) 0.9500 ? . . H(17) C(18) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 S(2) Mo(1) S(1) 78.86(3) ? . . . S(3) Mo(1) S(1) 85.99(4) ? . . . S(4) Mo(1) S(1) 158.75(5) ? . . . O(1) Mo(1) S(1) 111.1(1) ? . . . O(2) Mo(1) S(1) 82.0(1) ? . . . Mo(1) S(1) C(1) 111.6(1) ? . . . S(3) Mo(1) S(2) 85.72(4) ? . . . S(4) Mo(1) S(2) 84.89(3) ? . . . O(1) Mo(1) S(2) 87.7(1) ? . . . O(2) Mo(1) S(2) 160.4(1) ? . . . Mo(1) S(2) C(2) 108.2(1) ? . . . S(4) Mo(1) S(3) 79.18(3) ? . . . O(1) Mo(1) S(3) 160.1(1) ? . . . O(2) Mo(1) S(3) 88.8(1) ? . . . Mo(1) S(3) C(7) 108.5(1) ? . . . O(1) Mo(1) S(4) 81.6(1) ? . . . O(2) Mo(1) S(4) 112.6(1) ? . . . Mo(1) S(4) C(8) 110.8(1) ? . . . O(2) Mo(1) O(1) 103.2(1) ? . . . Cl(1) C(6) C(1) 119.2(3) ? . . . Cl(1) C(6) C(5) 117.4(3) ? . . . Cl(2) C(3) C(2) 119.7(3) ? . . . Cl(2) C(3) C(4) 117.4(3) ? . . . Cl(3) C(12) C(7) 118.8(3) ? . . . Cl(3) C(12) C(11) 117.8(3) ? . . . Cl(4) C(9) C(8) 119.2(3) ? . . . Cl(4) C(9) C(10) 117.9(3) ? . . . S(1) C(1) C(6) 121.0(3) ? . . . S(1) C(1) C(2) 121.1(3) ? . . . S(2) C(2) C(1) 120.2(3) ? . . . S(2) C(2) C(3) 121.8(3) ? . . . S(3) C(7) C(12) 121.6(3) ? . . . S(3) C(7) C(8) 120.5(3) ? . . . S(4) C(8) C(7) 120.9(3) ? . . . S(4) C(8) C(9) 121.0(3) ? . . . N(1) C(13) C(14) 115.8(5) ? . . . C(15) N(1) C(13) 110.4(4) ? . . . C(17) N(1) C(13) 110.7(4) ? . . . C(19) N(1) C(13) 107.5(5) ? . . . N(1) C(15) C(16) 114.6(4) ? . . . C(17) N(1) C(15) 106.0(4) ? . . . C(19) N(1) C(15) 111.3(4) ? . . . N(1) C(17) C(18) 114.7(5) ? . . . C(19) N(1) C(17) 111.0(4) ? . . . N(1) C(19) C(20) 114.3(7) ? . . . N(2) C(21) C(22) 114.6(3) ? . . . C(23) N(2) C(21) 110.9(3) ? . . . C(25) N(2) C(21) 111.4(3) ? . . . C(27) N(2) C(21) 107.0(3) ? . . . N(2) C(23) C(24) 115.9(3) ? . . . C(25) N(2) C(23) 106.4(3) ? . . . C(27) N(2) C(23) 110.5(3) ? . . . N(2) C(25) C(26) 115.2(4) ? . . . C(27) N(2) C(25) 110.7(3) ? . . . N(2) C(27) C(28) 114.8(4) ? . . . C(6) C(1) C(2) 117.9(3) ? . . . C(1) C(2) C(3) 117.9(3) ? . . . C(1) C(6) C(5) 123.4(3) ? . . . C(2) C(3) C(4) 122.8(4) ? . . . C(3) C(4) C(5) 119.3(4) ? . . . C(4) C(5) C(6) 118.7(4) ? . . . C(12) C(7) C(8) 117.8(4) ? . . . C(7) C(8) C(9) 118.1(3) ? . . . C(7) C(12) C(11) 123.3(4) ? . . . C(8) C(9) C(10) 122.9(4) ? . . . C(9) C(10) C(11) 119.4(4) ? . . . C(10) C(11) C(12) 118.5(4) ? . . . N(1) C(13) H(5) 108.0827 ? . . . N(1) C(13) H(6) 107.9123 ? . . . N(1) C(15) H(11) 108.0556 ? . . . N(1) C(15) H(10) 108.3206 ? . . . N(1) C(17) H(15) 108.4483 ? . . . N(1) C(17) H(16) 108.0057 ? . . . N(1) C(19) H(20) 108.3540 ? . . . N(1) C(19) H(21) 108.9403 ? . . . N(2) C(21) H(25) 108.0261 ? . . . N(2) C(21) H(26) 108.1982 ? . . . N(2) C(23) H(30) 108.0621 ? . . . N(2) C(23) H(31) 107.8271 ? . . . N(2) C(25) H(36) 108.1940 ? . . . N(2) C(25) H(35) 107.7216 ? . . . N(2) C(27) H(40) 108.2863 ? . . . N(2) C(27) H(41) 107.8992 ? . . . C(3) C(4) H(1) 120.1455 ? . . . C(4) C(5) H(2) 120.5800 ? . . . H(1) C(4) C(5) 120.5592 ? . . . H(2) C(5) C(6) 120.7413 ? . . . C(9) C(10) H(3) 120.0923 ? . . . C(10) C(11) H(4) 120.9890 ? . . . H(3) C(10) C(11) 120.4831 ? . . . H(4) C(11) C(12) 120.5529 ? . . . H(5) C(13) C(14) 107.1400 ? . . . H(6) C(13) C(14) 108.3402 ? . . . C(13) C(14) H(7) 108.7726 ? . . . C(13) C(14) H(9) 108.9687 ? . . . C(13) C(14) H(8) 110.6732 ? . . . H(6) C(13) H(5) 109.4521 ? . . . H(9) C(14) H(7) 109.4805 ? . . . H(8) C(14) H(7) 109.4658 ? . . . H(9) C(14) H(8) 109.4601 ? . . . H(11) C(15) C(16) 108.2337 ? . . . H(10) C(15) C(16) 108.1074 ? . . . C(15) C(16) H(12) 109.3888 ? . . . C(15) C(16) H(14) 109.1329 ? . . . C(15) C(16) H(13) 109.8782 ? . . . H(11) C(15) H(10) 109.4641 ? . . . H(14) C(16) H(12) 109.4905 ? . . . H(13) C(16) H(12) 109.4693 ? . . . H(14) C(16) H(13) 109.4668 ? . . . H(15) C(17) C(18) 109.0254 ? . . . H(16) C(17) C(18) 107.1080 ? . . . C(17) C(18) H(17) 110.5862 ? . . . C(17) C(18) H(19) 108.0383 ? . . . C(17) C(18) H(18) 109.7785 ? . . . H(16) C(17) H(15) 109.4599 ? . . . H(19) C(18) H(17) 109.4641 ? . . . H(18) C(18) H(17) 109.4742 ? . . . H(19) C(18) H(18) 109.4755 ? . . . H(20) C(19) C(20) 108.9384 ? . . . H(21) C(19) C(20) 106.8205 ? . . . C(19) C(20) H(22) 110.6920 ? . . . C(19) C(20) H(24) 107.3334 ? . . . C(19) C(20) H(23) 110.3660 ? . . . H(21) C(19) H(20) 109.4663 ? . . . H(24) C(20) H(22) 109.4790 ? . . . H(23) C(20) H(22) 109.4699 ? . . . H(24) C(20) H(23) 109.4652 ? . . . H(25) C(21) C(22) 108.0728 ? . . . H(26) C(21) C(22) 108.4224 ? . . . C(21) C(22) H(27) 109.2654 ? . . . C(21) C(22) H(29) 109.3063 ? . . . C(21) C(22) H(28) 109.8424 ? . . . H(26) C(21) H(25) 109.4565 ? . . . H(29) C(22) H(27) 109.4600 ? . . . H(28) C(22) H(27) 109.4724 ? . . . H(29) C(22) H(28) 109.4801 ? . . . H(30) C(23) C(24) 107.9771 ? . . . H(31) C(23) C(24) 107.5193 ? . . . C(23) C(24) H(32) 109.7403 ? . . . C(23) C(24) H(34) 108.7310 ? . . . C(23) C(24) H(33) 109.9375 ? . . . H(31) C(23) H(30) 109.4657 ? . . . H(34) C(24) H(32) 109.4677 ? . . . H(33) C(24) H(32) 109.4763 ? . . . H(34) C(24) H(33) 109.4718 ? . . . H(36) C(25) C(26) 108.3472 ? . . . H(35) C(25) C(26) 107.8197 ? . . . C(25) C(26) H(37) 109.1576 ? . . . C(25) C(26) H(39) 109.7207 ? . . . C(25) C(26) H(38) 109.5389 ? . . . H(36) C(25) H(35) 109.4557 ? . . . H(39) C(26) H(37) 109.4742 ? . . . H(38) C(26) H(37) 109.4692 ? . . . H(39) C(26) H(38) 109.4662 ? . . . C(27) C(28) H(42) 109.5046 ? . . . H(40) C(27) C(28) 108.1870 ? . . . H(41) C(27) C(28) 108.1392 ? . . . C(27) C(28) H(44) 109.3549 ? . . . C(27) C(28) H(43) 109.5596 ? . . . H(41) C(27) H(40) 109.4619 ? . . . H(44) C(28) H(42) 109.4724 ? . . . H(43) C(28) H(42) 109.4685 ? . . . H(44) C(28) H(43) 109.4673 ? . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 S(2) Mo(1) S(1) C(1) -1.0(1) ? . . . . S(3) Mo(1) S(1) C(1) -87.4(1) ? . . . . S(4) Mo(1) S(1) C(1) -41.8(2) ? . . . . O(1) Mo(1) S(1) C(1) 82.2(1) ? . . . . O(2) Mo(1) S(1) C(1) -176.8(1) ? . . . . S(1) Mo(1) S(2) C(2) 0.3(1) ? . . . . S(3) Mo(1) S(2) C(2) 87.0(1) ? . . . . S(4) Mo(1) S(2) C(2) 166.5(1) ? . . . . O(1) Mo(1) S(2) C(2) -111.8(1) ? . . . . O(2) Mo(1) S(2) C(2) 12.9(2) ? . . . . S(1) Mo(1) S(3) C(7) 163.7(1) ? . . . . S(2) Mo(1) S(3) C(7) 84.6(1) ? . . . . S(4) Mo(1) S(3) C(7) -1.0(1) ? . . . . O(1) Mo(1) S(3) C(7) 13.5(2) ? . . . . O(2) Mo(1) S(3) C(7) -114.2(1) ? . . . . S(1) Mo(1) S(4) C(8) -45.8(2) ? . . . . S(2) Mo(1) S(4) C(8) -85.9(1) ? . . . . S(3) Mo(1) S(4) C(8) 0.8(1) ? . . . . O(1) Mo(1) S(4) C(8) -174.3(1) ? . . . . O(2) Mo(1) S(4) C(8) 84.9(1) ? . . . . Mo(1) S(1) C(1) C(2) 1.9(3) ? . . . . Mo(1) S(1) C(1) C(6) -175.3(3) ? . . . . Mo(1) S(2) C(2) C(1) 0.7(3) ? . . . . Mo(1) S(2) C(2) C(3) 178.0(3) ? . . . . Mo(1) S(3) C(7) C(8) 1.1(3) ? . . . . Mo(1) S(3) C(7) C(12) 179.2(3) ? . . . . Mo(1) S(4) C(8) C(7) -0.4(3) ? . . . . Mo(1) S(4) C(8) C(9) 179.3(3) ? . . . . C(15) N(1) C(13) C(14) 54.8(6) ? . . . . C(17) N(1) C(13) C(14) -62.2(6) ? . . . . C(19) N(1) C(13) C(14) 176.4(5) ? . . . . C(13) N(1) C(15) C(16) 58.9(5) ? . . . . C(17) N(1) C(15) C(16) 178.8(4) ? . . . . C(19) N(1) C(15) C(16) -60.4(5) ? . . . . C(13) N(1) C(17) C(18) -57.9(6) ? . . . . C(15) N(1) C(17) C(18) -177.6(5) ? . . . . C(19) N(1) C(17) C(18) 61.4(6) ? . . . . C(13) N(1) C(19) C(20) -173.4(6) ? . . . . C(15) N(1) C(19) C(20) -52.4(7) ? . . . . C(17) N(1) C(19) C(20) 65.4(7) ? . . . . C(23) N(2) C(21) C(22) -56.6(4) ? . . . . C(25) N(2) C(21) C(22) 61.7(4) ? . . . . C(27) N(2) C(21) C(22) -177.2(3) ? . . . . C(21) N(2) C(23) C(24) -53.6(4) ? . . . . C(25) N(2) C(23) C(24) -174.9(3) ? . . . . C(27) N(2) C(23) C(24) 64.8(4) ? . . . . C(21) N(2) C(25) C(26) 63.8(4) ? . . . . C(23) N(2) C(25) C(26) -175.2(3) ? . . . . C(27) N(2) C(25) C(26) -55.0(4) ? . . . . C(21) N(2) C(27) C(28) -172.1(3) ? . . . . C(23) N(2) C(27) C(28) 67.1(4) ? . . . . C(25) N(2) C(27) C(28) -50.5(4) ? . . . . S(1) C(1) C(2) S(2) -1.7(5) ? . . . . S(1) C(1) C(2) C(3) -179.1(3) ? . . . . C(6) C(1) C(2) S(2) 175.5(3) ? . . . . C(6) C(1) C(2) C(3) -1.9(5) ? . . . . S(1) C(1) C(6) Cl(1) -1.0(5) ? . . . . S(1) C(1) C(6) C(5) 178.3(3) ? . . . . C(2) C(1) C(6) Cl(1) -178.3(3) ? . . . . C(2) C(1) C(6) C(5) 1.1(6) ? . . . . S(2) C(2) C(3) Cl(2) 4.3(5) ? . . . . S(2) C(2) C(3) C(4) -176.1(3) ? . . . . C(1) C(2) C(3) Cl(2) -178.4(3) ? . . . . C(1) C(2) C(3) C(4) 1.2(6) ? . . . . Cl(2) C(3) C(4) C(5) 180.0(2) ? . . . . C(2) C(3) C(4) C(5) 0.4(6) ? . . . . C(3) C(4) C(5) C(6) -1.3(6) ? . . . . C(4) C(5) C(6) Cl(1) 179.9(3) ? . . . . C(4) C(5) C(6) C(1) 0.5(6) ? . . . . S(3) C(7) C(8) S(4) -0.5(5) ? . . . . S(3) C(7) C(8) C(9) 179.8(3) ? . . . . C(12) C(7) C(8) S(4) -178.7(3) ? . . . . C(12) C(7) C(8) C(9) 1.6(5) ? . . . . S(3) C(7) C(12) Cl(3) -2.7(5) ? . . . . S(3) C(7) C(12) C(11) -179.7(4) ? . . . . C(8) C(7) C(12) Cl(3) 175.4(3) ? . . . . C(8) C(7) C(12) C(11) -1.5(6) ? . . . . S(4) C(8) C(9) Cl(4) 1.6(5) ? . . . . S(4) C(8) C(9) C(10) -179.9(3) ? . . . . C(7) C(8) C(9) Cl(4) -178.8(3) ? . . . . C(7) C(8) C(9) C(10) -0.3(6) ? . . . . Cl(4) C(9) C(10) C(11) 177.3(3) ? . . . . C(8) C(9) C(10) C(11) -1.3(6) ? . . . . C(9) C(10) C(11) C(12) 1.3(6) ? . . . . C(10) C(11) C(12) Cl(3) -177.0(3) ? . . . . C(10) C(11) C(12) C(7) 0.1(5) ? . . . . #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #============================================================================== data_(Et3NH)2[2] _database_code_depnum_ccdc_archive 'CCDC 253877' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H36 Cl4 N2 Mo O S4 ' _chemical_formula_moiety 'C24 H36 Cl4 N2 Mo O S4 ' _chemical_formula_weight 734.55 _chemical_melting_point ? _chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk' #============================================================================== # CRYSTAL DATA _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2+X,1/2-Y,-Z 3 -X,1/2+Y,1/2-Z 4 1/2-X,-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 7.822(4) _cell_length_b 16.049(7) _cell_length_c 25.348(12) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3182.1(25) _cell_formula_units_Z 4 _cell_measurement_reflns_used 10750 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 123 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504.00 _exptl_absorpt_coefficient_mu 1.031 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.554 _exptl_absorpt_correction_T_max 0.940 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 25288 _diffrn_reflns_av_R_equivalents 0.067 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9915 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9915 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 28 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 7247 _reflns_number_gt 6569 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1580 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 7247 _refine_ls_number_parameters 362 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0028Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 4.10 _refine_diff_density_min -2.12 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack, H. D. (1983), Acta Cryst. A39, 876-881. 3115 Friedel Pairs' _refine_ls_abs_structure_Flack 0.12(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mo Mo -1.683 0.686 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo(1) Mo 0.21939(6) 0.05053(3) 0.37635(2) 0.02022(10) Uani 1.00 1 d . . . Cl(1) Cl 0.1817(2) 0.03402(10) 0.59299(5) 0.0332(4) Uani 1.00 1 d . . . Cl(2) Cl -0.0315(2) -0.25387(9) 0.44206(6) 0.0369(4) Uani 1.00 1 d . . . Cl(3) Cl 0.0230(2) 0.08185(10) 0.16889(6) 0.0359(4) Uani 1.00 1 d . . . Cl(4) Cl -0.0171(2) 0.36766(9) 0.33421(6) 0.0357(4) Uani 1.00 1 d . . . S(1) S 0.1803(2) 0.06792(8) 0.46856(5) 0.0227(3) Uani 1.00 1 d . . . S(2) S 0.0987(2) -0.08225(8) 0.39177(5) 0.0233(3) Uani 1.00 1 d . . . S(3) S 0.0996(2) 0.03969(8) 0.29094(5) 0.0227(3) Uani 1.00 1 d . . . S(4) S 0.1187(2) 0.18934(8) 0.37172(5) 0.0236(3) Uani 1.00 1 d . . . O(1) O 0.4371(5) 0.0444(3) 0.3675(2) 0.0286(10) Uani 1.00 1 d . . . N(1) N 0.5555(7) -0.0386(4) 0.2771(2) 0.034(1) Uani 1.00 1 d . . . N(2) N 0.6176(6) 0.0863(3) 0.4676(2) 0.0268(12) Uani 1.00 1 d . . . C(1) C 0.1320(6) -0.0317(4) 0.4947(2) 0.0241(13) Uani 1.00 1 d . . . C(2) C 0.0912(7) -0.0969(4) 0.4606(2) 0.0237(13) Uani 1.00 1 d . . . C(3) C 0.0331(7) -0.1721(4) 0.4832(2) 0.026(1) Uani 1.00 1 d . . . C(4) C 0.0217(9) -0.1837(4) 0.5368(2) 0.033(2) Uani 1.00 1 d . . . C(5) C 0.0688(9) -0.1202(4) 0.5713(2) 0.034(2) Uani 1.00 1 d . . . C(6) C 0.1247(7) -0.0447(4) 0.5495(2) 0.0266(13) Uani 1.00 1 d . . . C(7) C 0.0537(7) 0.1420(3) 0.2691(2) 0.0226(13) Uani 1.00 1 d . . . C(8) C 0.0530(7) 0.2074(3) 0.3056(2) 0.0242(13) Uani 1.00 1 d . . . C(9) C -0.0013(7) 0.2862(3) 0.2892(2) 0.0250(13) Uani 1.00 1 d . . . C(10) C -0.0453(8) 0.3033(4) 0.2371(2) 0.027(1) Uani 1.00 1 d . . . C(11) C -0.0392(8) 0.2385(4) 0.1996(2) 0.029(1) Uani 1.00 1 d . . . C(12) C 0.0112(7) 0.1605(4) 0.2170(2) 0.0256(13) Uani 1.00 1 d . . . C(13) C 0.6456(10) 0.0300(6) 0.2481(3) 0.053(2) Uani 1.00 1 d . . . C(14) C 0.5274(13) 0.0951(8) 0.2282(4) 0.083(4) Uani 1.00 1 d . . . C(15) C 0.6863(8) -0.0869(5) 0.3083(3) 0.040(2) Uani 1.00 1 d . . . C(16) C 0.6070(11) -0.1541(5) 0.3427(3) 0.049(2) Uani 1.00 1 d . . . C(17) C 0.4425(9) -0.0935(5) 0.2437(3) 0.040(2) Uani 1.00 1 d . . . C(18) C 0.5373(13) -0.1473(7) 0.2046(4) 0.072(3) Uani 1.00 1 d . . . C(19) C 0.6942(7) 0.0004(4) 0.4621(3) 0.031(2) Uani 1.00 1 d . . . C(20) C 0.5948(9) -0.0663(5) 0.4918(3) 0.043(2) Uani 1.00 1 d . . . C(21) C 0.6024(8) 0.1164(4) 0.5231(3) 0.036(2) Uani 1.00 1 d . . . C(22) C 0.7706(10) 0.1164(6) 0.5519(3) 0.057(2) Uani 1.00 1 d . . . C(23) C 0.7161(9) 0.1443(4) 0.4308(3) 0.038(2) Uani 1.00 1 d . . . C(24) C 0.6332(12) 0.2293(5) 0.4265(4) 0.060(3) Uani 1.00 1 d . . . H(1) H 0.4839 -0.0123 0.3024 0.041 Uiso 1.00 1 c R . . H(2) H 0.5046 0.0831 0.4540 0.032 Uiso 1.00 1 c R . . H(3) H -0.0193 -0.2352 0.5503 0.040 Uiso 1.00 1 c R . . H(4) H 0.0638 -0.1279 0.6084 0.041 Uiso 1.00 1 c R . . H(5) H -0.0793 0.3578 0.2270 0.032 Uiso 1.00 1 c R . . H(6) H -0.0685 0.2477 0.1637 0.034 Uiso 1.00 1 c R . . H(7) H 0.7240 0.0561 0.2714 0.063 Uiso 1.00 1 c R . . H(8) H 0.7060 0.0069 0.2190 0.063 Uiso 1.00 1 c R . . H(9) H 0.4909 0.0801 0.1937 0.100 Uiso 1.00 1 c R . . H(10) H 0.5815 0.1480 0.2271 0.100 Uiso 1.00 1 c R . . H(11) H 0.4314 0.0975 0.2511 0.100 Uiso 1.00 1 c R . . H(12) H 0.7633 -0.1125 0.2843 0.049 Uiso 1.00 1 c R . . H(13) H 0.7472 -0.0493 0.3303 0.048 Uiso 1.00 1 c R . . H(14) H 0.5809 -0.1316 0.3764 0.059 Uiso 1.00 1 c R . . H(15) H 0.6846 -0.1992 0.3466 0.059 Uiso 1.00 1 c R . . H(16) H 0.5051 -0.1734 0.3264 0.059 Uiso 1.00 1 c R . . H(17) H 0.5480 -0.1182 0.1721 0.086 Uiso 1.00 1 c R . . H(18) H 0.4775 -0.1980 0.1989 0.086 Uiso 1.00 1 c R . . H(19) H 0.6479 -0.1591 0.2182 0.086 Uiso 1.00 1 c R . . H(20) H 0.3812 -0.1293 0.2669 0.048 Uiso 1.00 1 c R . . H(21) H 0.3642 -0.0596 0.2248 0.048 Uiso 1.00 1 c R . . H(22) H 0.6948 -0.0138 0.4257 0.037 Uiso 1.00 1 c R . . H(23) H 0.8083 0.0017 0.4749 0.037 Uiso 1.00 1 c R . . H(24) H 0.6397 -0.0711 0.5265 0.052 Uiso 1.00 1 c R . . H(25) H 0.6052 -0.1182 0.4741 0.052 Uiso 1.00 1 c R . . H(26) H 0.4776 -0.0509 0.4936 0.052 Uiso 1.00 1 c R . . H(27) H 0.5640 0.1725 0.5222 0.043 Uiso 1.00 1 c R . . H(28) H 0.5214 0.0832 0.5415 0.043 Uiso 1.00 1 c R . . H(29) H 0.7813 0.0641 0.5691 0.068 Uiso 1.00 1 c R . . H(30) H 0.7746 0.1598 0.5774 0.068 Uiso 1.00 1 c R . . H(31) H 0.8618 0.1232 0.5275 0.068 Uiso 1.00 1 c R . . H(32) H 0.8295 0.1504 0.4437 0.046 Uiso 1.00 1 c R . . H(33) H 0.7189 0.1203 0.3966 0.046 Uiso 1.00 1 c R . . H(34) H 0.5518 0.2297 0.3986 0.073 Uiso 1.00 1 c R . . H(35) H 0.7178 0.2705 0.4199 0.073 Uiso 1.00 1 c R . . H(36) H 0.5774 0.2410 0.4589 0.073 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mo(1) 0.0196(2) 0.0181(2) 0.0230(2) 0.0013(2) -0.0004(2) -0.0002(2) Cl(1) 0.0409(8) 0.0355(8) 0.0233(6) 0.0021(6) -0.0051(5) -0.0042(5) Cl(2) 0.0570(10) 0.0211(7) 0.0325(7) -0.0075(6) -0.0044(7) 0.0039(6) Cl(3) 0.0602(10) 0.0250(7) 0.0225(6) 0.0037(7) 0.0012(6) -0.0018(5) Cl(4) 0.0493(9) 0.0199(6) 0.0380(8) 0.0082(6) -0.0036(6) -0.0044(6) S(1) 0.0222(6) 0.0230(6) 0.0229(6) 0.0009(5) -0.0008(4) -0.0022(5) S(2) 0.0307(7) 0.0168(6) 0.0226(6) -0.0019(5) -0.0027(5) 0.0004(5) S(3) 0.0268(6) 0.0186(6) 0.0227(6) -0.0008(5) -0.0013(5) -0.0007(5) S(4) 0.0285(6) 0.0175(6) 0.0249(6) 0.0030(4) -0.0011(5) -0.0014(5) O(1) 0.023(2) 0.033(2) 0.029(2) 0.003(2) -0.002(1) -0.002(2) N(1) 0.031(3) 0.042(3) 0.030(3) -0.001(2) 0.005(2) -0.001(2) N(2) 0.017(2) 0.025(2) 0.038(3) 0.002(2) -0.001(2) 0.000(2) C(1) 0.017(2) 0.030(3) 0.025(3) 0.001(2) -0.000(2) 0.002(2) C(2) 0.021(2) 0.027(3) 0.023(2) -0.001(2) -0.001(2) -0.004(2) C(3) 0.026(3) 0.027(3) 0.024(3) -0.001(2) 0.005(2) 0.004(2) C(4) 0.044(4) 0.029(3) 0.026(3) -0.005(3) 0.001(2) 0.005(2) C(5) 0.043(4) 0.037(3) 0.022(3) 0.006(3) -0.001(3) 0.007(2) C(6) 0.027(3) 0.025(3) 0.028(3) 0.003(2) -0.001(2) -0.003(2) C(7) 0.020(3) 0.020(3) 0.027(3) -0.000(2) 0.006(2) 0.000(2) C(8) 0.022(3) 0.022(3) 0.029(3) -0.003(2) 0.004(2) -0.001(2) C(9) 0.026(3) 0.019(3) 0.030(3) -0.001(2) 0.002(2) 0.001(2) C(10) 0.030(3) 0.019(3) 0.032(3) 0.002(2) 0.004(2) 0.008(2) C(11) 0.030(3) 0.028(3) 0.028(3) 0.000(2) -0.001(2) 0.007(2) C(12) 0.025(3) 0.023(3) 0.029(3) -0.000(2) 0.006(2) -0.001(2) C(13) 0.042(4) 0.062(5) 0.054(5) -0.006(4) 0.013(3) 0.016(4) C(14) 0.051(5) 0.107(9) 0.091(8) -0.002(6) 0.007(5) 0.066(7) C(15) 0.023(3) 0.052(4) 0.046(4) 0.002(3) 0.006(3) -0.016(3) C(16) 0.049(4) 0.049(5) 0.048(4) 0.014(4) -0.006(3) 0.005(3) C(17) 0.029(3) 0.046(4) 0.045(4) 0.009(3) -0.004(3) -0.013(3) C(18) 0.061(6) 0.083(7) 0.070(6) 0.036(5) -0.018(5) -0.047(6) C(19) 0.025(3) 0.025(3) 0.043(3) 0.001(2) -0.001(2) -0.006(2) C(20) 0.036(4) 0.035(4) 0.058(4) -0.000(3) -0.006(3) 0.010(3) C(21) 0.024(3) 0.037(4) 0.046(4) 0.003(2) 0.002(3) -0.004(3) C(22) 0.035(4) 0.098(7) 0.037(4) 0.004(4) -0.005(3) -0.035(4) C(23) 0.029(3) 0.035(3) 0.050(4) -0.008(3) -0.001(3) 0.005(3) C(24) 0.062(6) 0.032(4) 0.088(7) -0.011(4) -0.019(5) 0.014(4) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution SIR97 _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mo(1) S(1) 2.374(1) ? . . Mo(1) S(2) 2.363(1) ? . . Mo(1) S(3) 2.365(1) ? . . Mo(1) S(4) 2.366(1) ? . . Mo(1) O(1) 1.720(4) ? . . Cl(1) C(6) 1.736(6) ? . . Cl(2) C(3) 1.751(6) ? . . Cl(3) C(12) 1.758(6) ? . . Cl(4) C(9) 1.739(6) ? . . S(1) C(1) 1.771(6) ? . . S(2) C(2) 1.760(5) ? . . S(3) C(7) 1.770(6) ? . . S(4) C(8) 1.777(6) ? . . N(1) C(13) 1.50(1) ? . . N(1) C(15) 1.508(9) ? . . N(1) C(17) 1.508(9) ? . . N(2) C(19) 1.510(8) ? . . N(2) C(21) 1.493(9) ? . . N(2) C(23) 1.525(8) ? . . C(1) C(2) 1.394(8) ? . . C(1) C(6) 1.406(8) ? . . C(2) C(3) 1.412(8) ? . . C(3) C(4) 1.375(8) ? . . C(4) C(5) 1.392(9) ? . . C(5) C(6) 1.401(9) ? . . C(6) Cl(1) 1.736(6) ? . . C(6) C(1) 1.406(8) ? . . C(6) C(5) 1.401(9) ? . . C(7) C(8) 1.400(8) ? . . C(7) C(12) 1.393(8) ? . . C(8) C(9) 1.397(8) ? . . C(9) C(10) 1.393(8) ? . . C(10) C(11) 1.409(8) ? . . C(11) C(12) 1.385(8) ? . . C(13) C(14) 1.48(1) ? . . C(15) C(16) 1.52(1) ? . . C(17) C(18) 1.51(1) ? . . C(19) C(20) 1.522(9) ? . . C(21) C(22) 1.50(1) ? . . C(23) C(24) 1.51(1) ? . . N(1) H(1) 0.9500 ? . . N(2) H(2) 0.9500 ? . . C(4) H(3) 0.9501 ? . . C(5) H(4) 0.9500 ? . . C(10) H(5) 0.9500 ? . . C(11) H(6) 0.9501 ? . . C(13) H(7) 0.9500 ? . . C(13) H(8) 0.9499 ? . . C(14) H(9) 0.9499 ? . . C(14) H(10) 0.9500 ? . . C(14) H(11) 0.9500 ? . . C(15) H(12) 0.9499 ? . . C(15) H(13) 0.9500 ? . . C(16) H(14) 0.9500 ? . . C(16) H(15) 0.9500 ? . . C(16) H(16) 0.9499 ? . . C(17) H(20) 0.9499 ? . . C(17) H(21) 0.9500 ? . . C(18) H(17) 0.9500 ? . . C(18) H(18) 0.9501 ? . . C(18) H(19) 0.9501 ? . . C(19) H(22) 0.9499 ? . . C(19) H(23) 0.9500 ? . . C(20) H(24) 0.9501 ? . . C(20) H(25) 0.9499 ? . . C(20) H(26) 0.9500 ? . . C(21) H(27) 0.9500 ? . . C(21) H(28) 0.9500 ? . . C(22) H(29) 0.9501 ? . . C(22) H(30) 0.9499 ? . . C(22) H(31) 0.9501 ? . . C(23) H(32) 0.9500 ? . . C(23) H(33) 0.9500 ? . . C(24) H(34) 0.9500 ? . . C(24) H(35) 0.9500 ? . . C(24) H(36) 0.9500 ? . . H(23) C(19) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 S(2) Mo(1) S(1) 83.78(5) ? . . . S(3) Mo(1) S(1) 149.19(5) ? . . . S(4) Mo(1) S(1) 83.99(5) ? . . . O(1) Mo(1) S(1) 105.2(1) ? . . . Mo(1) S(1) C(1) 106.8(2) ? . . . S(3) Mo(1) S(2) 85.81(5) ? . . . S(4) Mo(1) S(2) 136.42(5) ? . . . O(1) Mo(1) S(2) 111.4(2) ? . . . Mo(1) S(2) C(2) 107.3(2) ? . . . S(4) Mo(1) S(3) 83.80(5) ? . . . O(1) Mo(1) S(3) 105.6(1) ? . . . Mo(1) S(3) C(7) 107.4(2) ? . . . O(1) Mo(1) S(4) 112.2(1) ? . . . Mo(1) S(4) C(8) 107.3(2) ? . . . Cl(1) C(6) C(1) 120.6(4) ? . . . Cl(1) C(6) C(5) 117.3(4) ? . . . Cl(2) C(3) C(2) 119.4(4) ? . . . Cl(2) C(3) C(4) 117.9(5) ? . . . Cl(3) C(12) C(7) 119.5(4) ? . . . Cl(3) C(12) C(11) 116.3(4) ? . . . Cl(4) C(9) C(8) 120.5(4) ? . . . Cl(4) C(9) C(10) 117.2(4) ? . . . S(1) C(1) C(2) 119.6(4) ? . . . S(1) C(1) C(6) 120.8(4) ? . . . S(2) C(2) C(1) 120.5(4) ? . . . S(2) C(2) C(3) 121.8(4) ? . . . S(3) C(7) C(8) 119.3(4) ? . . . S(3) C(7) C(12) 122.9(4) ? . . . S(4) C(8) C(7) 120.0(4) ? . . . S(4) C(8) C(9) 121.1(4) ? . . . C(15) N(1) C(13) 108.4(5) ? . . . N(1) C(13) C(14) 113.0(7) ? . . . C(17) N(1) C(13) 115.4(5) ? . . . N(1) C(15) C(16) 112.9(5) ? . . . C(17) N(1) C(15) 113.0(6) ? . . . N(1) C(17) C(18) 114.5(6) ? . . . C(23) N(2) C(19) 107.5(4) ? . . . N(2) C(19) C(20) 113.2(5) ? . . . C(21) N(2) C(19) 114.4(5) ? . . . C(23) N(2) C(21) 114.8(5) ? . . . N(2) C(21) C(22) 112.8(5) ? . . . N(2) C(23) C(24) 112.2(6) ? . . . C(6) C(1) C(2) 119.5(5) ? . . . C(1) C(2) C(3) 117.6(5) ? . . . C(1) C(6) C(5) 122.1(5) ? . . . C(2) C(3) C(4) 122.6(6) ? . . . C(3) C(4) C(5) 120.2(6) ? . . . C(4) C(5) C(6) 117.9(6) ? . . . C(12) C(7) C(8) 117.8(5) ? . . . C(7) C(8) C(9) 118.9(5) ? . . . C(7) C(12) C(11) 124.2(5) ? . . . C(8) C(9) C(10) 122.4(5) ? . . . C(9) C(10) C(11) 119.1(5) ? . . . C(10) C(11) C(12) 117.5(5) ? . . . H(1) N(1) C(13) 106.4057 ? . . . N(1) C(13) H(7) 108.7734 ? . . . N(1) C(13) H(8) 109.1277 ? . . . H(1) N(1) C(15) 105.9166 ? . . . N(1) C(15) H(13) 108.7622 ? . . . N(1) C(15) H(12) 108.4018 ? . . . H(1) N(1) C(17) 106.9665 ? . . . N(1) C(17) H(20) 107.6206 ? . . . N(1) C(17) H(21) 109.0158 ? . . . H(2) N(2) C(19) 106.6196 ? . . . N(2) C(19) H(22) 108.1212 ? . . . N(2) C(19) H(23) 108.7368 ? . . . H(2) N(2) C(21) 106.6080 ? . . . N(2) C(21) H(28) 109.4749 ? . . . N(2) C(21) H(27) 107.9971 ? . . . H(2) N(2) C(23) 106.3507 ? . . . N(2) C(23) H(33) 108.7868 ? . . . N(2) C(23) H(32) 108.9754 ? . . . C(3) C(4) H(3) 119.6769 ? . . . C(4) C(5) H(4) 121.0394 ? . . . H(3) C(4) C(5) 120.0947 ? . . . H(4) C(5) C(6) 121.0610 ? . . . C(9) C(10) H(5) 120.4367 ? . . . C(10) C(11) H(6) 121.5520 ? . . . H(5) C(10) C(11) 120.4591 ? . . . H(6) C(11) C(12) 120.9368 ? . . . C(13) C(14) H(11) 108.3279 ? . . . H(7) C(13) C(14) 107.6449 ? . . . H(8) C(13) C(14) 108.7785 ? . . . C(13) C(14) H(9) 108.8018 ? . . . C(13) C(14) H(10) 111.2633 ? . . . H(8) C(13) H(7) 109.4568 ? . . . H(11) C(14) H(9) 109.4742 ? . . . H(10) C(14) H(9) 109.4803 ? . . . H(11) C(14) H(10) 109.4648 ? . . . H(13) C(15) C(16) 108.5745 ? . . . C(15) C(16) H(14) 109.5445 ? . . . H(12) C(15) C(16) 108.6965 ? . . . C(15) C(16) H(15) 109.9087 ? . . . C(15) C(16) H(16) 108.9548 ? . . . H(13) C(15) H(12) 109.4618 ? . . . H(15) C(16) H(14) 109.4737 ? . . . H(16) C(16) H(14) 109.4676 ? . . . H(16) C(16) H(15) 109.4766 ? . . . H(20) C(17) C(18) 107.9864 ? . . . H(21) C(17) C(18) 108.1959 ? . . . C(17) C(18) H(17) 109.3459 ? . . . C(17) C(18) H(18) 110.3308 ? . . . C(17) C(18) H(19) 108.7259 ? . . . H(21) C(17) H(20) 109.4601 ? . . . H(18) C(18) H(17) 109.4742 ? . . . H(19) C(18) H(17) 109.4749 ? . . . H(19) C(18) H(18) 109.4716 ? . . . C(19) C(20) H(26) 109.5120 ? . . . H(22) C(19) C(20) 108.2632 ? . . . H(23) C(19) C(20) 109.0094 ? . . . C(19) C(20) H(24) 109.0396 ? . . . C(19) C(20) H(25) 109.8573 ? . . . H(23) C(19) H(22) 109.4565 ? . . . H(26) C(20) H(24) 109.4705 ? . . . H(25) C(20) H(24) 109.4745 ? . . . H(26) C(20) H(25) 109.4724 ? . . . H(28) C(21) C(22) 110.2513 ? . . . H(27) C(21) C(22) 106.7483 ? . . . C(21) C(22) H(29) 107.4373 ? . . . C(21) C(22) H(30) 111.0038 ? . . . C(21) C(22) H(31) 109.9421 ? . . . H(28) C(21) H(27) 109.4648 ? . . . H(30) C(22) H(29) 109.4756 ? . . . H(31) C(22) H(29) 109.4789 ? . . . H(31) C(22) H(30) 109.4688 ? . . . C(23) C(24) H(34) 110.2768 ? . . . H(33) C(23) C(24) 107.9780 ? . . . H(32) C(23) C(24) 109.3739 ? . . . C(23) C(24) H(35) 109.9826 ? . . . C(23) C(24) H(36) 108.1459 ? . . . H(33) C(23) H(32) 109.4605 ? . . . H(35) C(24) H(34) 109.4788 ? . . . H(36) C(24) H(34) 109.4655 ? . . . H(36) C(24) H(35) 109.4692 ? . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 S(2) Mo(1) S(1) C(1) 12.3(2) ? . . . . S(3) Mo(1) S(1) C(1) 83.3(2) ? . . . . S(4) Mo(1) S(1) C(1) 150.4(2) ? . . . . O(1) Mo(1) S(1) C(1) -98.2(2) ? . . . . S(1) Mo(1) S(2) C(2) -11.0(2) ? . . . . S(3) Mo(1) S(2) C(2) -162.0(2) ? . . . . S(4) Mo(1) S(2) C(2) -85.5(2) ? . . . . O(1) Mo(1) S(2) C(2) 92.9(2) ? . . . . S(1) Mo(1) S(3) C(7) 80.2(2) ? . . . . S(2) Mo(1) S(3) C(7) 150.6(2) ? . . . . S(4) Mo(1) S(3) C(7) 13.0(2) ? . . . . O(1) Mo(1) S(3) C(7) -98.3(2) ? . . . . S(1) Mo(1) S(4) C(8) -162.0(2) ? . . . . S(2) Mo(1) S(4) C(8) -87.6(2) ? . . . . S(3) Mo(1) S(4) C(8) -10.4(2) ? . . . . O(1) Mo(1) S(4) C(8) 94.0(2) ? . . . . Mo(1) S(1) C(1) C(2) -12.5(5) ? . . . . Mo(1) S(1) C(1) C(6) 171.2(4) ? . . . . Mo(1) S(2) C(2) C(1) 7.5(5) ? . . . . Mo(1) S(2) C(2) C(3) -176.9(4) ? . . . . Mo(1) S(3) C(7) C(8) -14.6(5) ? . . . . Mo(1) S(3) C(7) C(12) 168.0(4) ? . . . . Mo(1) S(4) C(8) C(7) 5.3(5) ? . . . . Mo(1) S(4) C(8) C(9) -175.2(4) ? . . . . C(15) N(1) C(13) C(14) -164.1(7) ? . . . . C(17) N(1) C(13) C(14) 67.9(9) ? . . . . C(13) N(1) C(15) C(16) 175.6(6) ? . . . . C(17) N(1) C(15) C(16) -55.1(7) ? . . . . C(13) N(1) C(17) C(18) 67.7(8) ? . . . . C(15) N(1) C(17) C(18) -57.9(8) ? . . . . C(21) N(2) C(19) C(20) 58.1(6) ? . . . . C(23) N(2) C(19) C(20) -173.2(5) ? . . . . C(19) N(2) C(21) C(22) 56.5(7) ? . . . . C(23) N(2) C(21) C(22) -68.4(7) ? . . . . C(19) N(2) C(23) C(24) 171.0(6) ? . . . . C(21) N(2) C(23) C(24) -60.5(7) ? . . . . S(1) C(1) C(2) S(2) 3.5(7) ? . . . . S(1) C(1) C(2) C(3) -172.3(4) ? . . . . C(6) C(1) C(2) S(2) 179.8(4) ? . . . . C(6) C(1) C(2) C(3) 4.1(8) ? . . . . S(1) C(1) C(6) Cl(1) -5.9(7) ? . . . . S(1) C(1) C(6) C(5) 172.9(5) ? . . . . C(2) C(1) C(6) Cl(1) 177.8(4) ? . . . . C(2) C(1) C(6) C(5) -3.4(8) ? . . . . S(2) C(2) C(3) Cl(2) 0.7(7) ? . . . . S(2) C(2) C(3) C(4) -178.0(5) ? . . . . C(1) C(2) C(3) Cl(2) 176.4(4) ? . . . . C(1) C(2) C(3) C(4) -2.3(9) ? . . . . Cl(2) C(3) C(4) C(5) -179.0(6) ? . . . . C(2) C(3) C(4) C(5) -0.3(8) ? . . . . C(3) C(4) C(5) C(6) 1(1) ? . . . . C(4) C(5) C(6) Cl(1) 179.6(5) ? . . . . C(4) C(5) C(6) C(1) 0.8(9) ? . . . . S(3) C(7) C(8) S(4) 6.4(7) ? . . . . S(3) C(7) C(8) C(9) -173.1(5) ? . . . . C(12) C(7) C(8) S(4) -176.1(4) ? . . . . C(12) C(7) C(8) C(9) 4.4(8) ? . . . . S(3) C(7) C(12) Cl(3) -6.5(7) ? . . . . S(3) C(7) C(12) C(11) 174.3(5) ? . . . . C(8) C(7) C(12) Cl(3) 176.1(4) ? . . . . C(8) C(7) C(12) C(11) -3.1(9) ? . . . . S(4) C(8) C(9) Cl(4) -3.5(7) ? . . . . S(4) C(8) C(9) C(10) 176.7(5) ? . . . . C(7) C(8) C(9) Cl(4) 176.0(4) ? . . . . C(7) C(8) C(9) C(10) -3.9(9) ? . . . . Cl(4) C(9) C(10) C(11) -178.2(5) ? . . . . C(8) C(9) C(10) C(11) 1.7(9) ? . . . . C(9) C(10) C(11) C(12) -0.1(7) ? . . . . C(10) C(11) C(12) Cl(3) -178.3(5) ? . . . . C(10) C(11) C(12) C(7) 0.9(9) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Mo(1) C(1) 3.347(5) ? . . Mo(1) C(2) 3.340(6) ? . . Mo(1) C(7) 3.351(5) ? . . Mo(1) C(8) 3.354(6) ? . . Cl(1) Cl(3) 3.535(2) ? . 55504 Cl(1) Cl(4) 3.383(2) ? . 55602 Cl(1) S(1) 3.201(2) ? . . Cl(1) C(1) 2.734(6) ? . . Cl(1) C(5) 2.685(7) ? . . Cl(2) S(2) 3.201(2) ? . . Cl(2) C(2) 2.737(6) ? . . Cl(2) C(4) 2.686(6) ? . . Cl(2) C(20) 3.481(8) ? . 44602 Cl(3) Cl(1) 3.535(2) ? . 55404 Cl(3) Cl(4) 3.439(2) ? . 54503 Cl(3) S(3) 3.223(2) ? . . Cl(3) C(7) 2.727(6) ? . . Cl(3) C(11) 2.677(6) ? . . Cl(4) Cl(1) 3.383(2) ? . 45602 Cl(4) Cl(3) 3.439(2) ? . 55503 Cl(4) S(4) 3.197(2) ? . . Cl(4) C(8) 2.728(6) ? . . Cl(4) C(10) 2.680(6) ? . . S(1) S(2) 3.163(2) ? . . S(1) S(4) 3.171(2) ? . . S(1) O(1) 3.276(4) ? . . S(1) N(2) 3.434(5) ? . . S(1) C(2) 2.742(6) ? . . S(1) C(6) 2.769(6) ? . . S(2) S(3) 3.219(2) ? . . S(2) O(1) 3.393(4) ? . . S(2) C(1) 2.744(6) ? . . S(2) C(3) 2.777(6) ? . . S(3) S(4) 3.160(2) ? . . S(3) O(1) 3.278(4) ? . . S(3) C(8) 2.742(6) ? . . S(3) C(12) 2.784(6) ? . . S(4) O(1) 3.410(4) ? . . S(4) C(7) 2.758(5) ? . . S(4) C(9) 2.769(6) ? . . S(4) C(23) 3.562(7) ? . 45501 O(1) N(1) 2.809(7) ? . . O(1) N(2) 2.979(6) ? . . O(1) C(13) 3.448(9) ? . . O(1) C(15) 3.240(8) ? . . O(1) C(16) 3.508(9) ? . . O(1) C(19) 3.207(7) ? . . O(1) C(23) 3.148(8) ? . . N(1) C(14) 2.49(1) ? . . N(1) C(16) 2.52(1) ? . . N(1) C(18) 2.54(1) ? . . N(2) C(20) 2.531(9) ? . . N(2) C(22) 2.497(9) ? . . N(2) C(24) 2.52(1) ? . . C(1) C(3) 2.400(8) ? . . C(1) C(4) 2.800(9) ? . . C(1) C(5) 2.457(9) ? . . C(1) C(19) 3.560(8) ? . 45501 C(2) C(4) 2.445(8) ? . . C(2) C(5) 2.837(8) ? . . C(2) C(6) 2.419(8) ? . . C(2) C(19) 3.476(8) ? . 45501 C(3) C(5) 2.399(8) ? . . C(3) C(6) 2.741(8) ? . . C(4) C(6) 2.393(9) ? . . C(6) S(1) 2.769(6) ? . . C(6) C(2) 2.419(8) ? . . C(6) C(3) 2.741(8) ? . . C(6) C(4) 2.393(9) ? . . C(7) C(9) 2.408(8) ? . . C(7) C(10) 2.820(8) ? . . C(7) C(11) 2.455(8) ? . . C(8) C(10) 2.444(8) ? . . C(8) C(11) 2.827(8) ? . . C(8) C(12) 2.391(8) ? . . C(9) C(11) 2.416(8) ? . . C(9) C(12) 2.726(8) ? . . C(10) C(12) 2.388(8) ? . . C(10) C(15) 3.509(9) ? . 65503 C(10) C(17) 3.554(9) ? . 55503 C(13) C(15) 2.44(1) ? . . C(13) C(17) 2.54(1) ? . . C(13) C(18) 3.17(1) ? . . C(14) C(17) 3.12(1) ? . . C(15) C(10) 3.509(9) ? . 64503 C(15) C(17) 2.52(1) ? . . C(15) C(18) 3.04(1) ? . . C(16) C(17) 2.98(1) ? . . C(16) C(18) 3.55(1) ? . . C(17) C(10) 3.554(9) ? . 54503 C(19) C(1) 3.560(8) ? . 65501 C(19) C(2) 3.476(8) ? . 65501 C(19) C(21) 2.524(9) ? . . C(19) C(22) 3.00(1) ? . . C(19) C(23) 2.447(9) ? . . C(20) Cl(2) 3.481(8) ? . 54602 C(20) C(21) 3.04(1) ? . . C(20) C(22) 3.58(1) ? . . C(21) C(23) 2.54(1) ? . . C(21) C(24) 3.06(1) ? . . C(22) C(23) 3.13(1) ? . . C(23) S(4) 3.562(7) ? . 65501 Mo(1) H(1) 2.9687 ? . . Mo(1) H(2) 3.0204 ? . . Cl(1) H(4) 2.7851 ? . . Cl(1) H(9) 3.4205 ? . 55504 Cl(1) H(17) 3.0122 ? . 55504 Cl(1) H(21) 3.3853 ? . 55504 Cl(1) H(28) 3.0636 ? . . Cl(1) H(29) 3.2261 ? . 45501 Cl(1) H(31) 3.3260 ? . 45501 Cl(1) H(35) 3.1665 ? . 45602 Cl(2) H(3) 2.7613 ? . . Cl(2) H(6) 2.7924 ? . 54503 Cl(2) H(15) 3.3989 ? . 45501 Cl(2) H(24) 3.2123 ? . 44602 Cl(2) H(25) 3.1417 ? . 44602 Cl(2) H(26) 3.5326 ? . 44602 Cl(3) H(6) 2.7597 ? . . Cl(3) H(7) 3.5201 ? . 45501 Cl(3) H(8) 3.0344 ? . 45501 Cl(4) H(5) 2.7667 ? . . Cl(4) H(8) 3.5688 ? . 65503 Cl(4) H(19) 3.2078 ? . 65503 Cl(4) H(21) 3.3126 ? . 55503 Cl(4) H(28) 3.2620 ? . 45602 Cl(4) H(29) 3.5570 ? . 45602 Cl(4) H(30) 3.2289 ? . 45602 Cl(4) H(35) 3.3840 ? . 45501 S(1) H(2) 2.5755 ? . . S(1) H(23) 3.1019 ? . 45501 S(1) H(26) 3.0742 ? . . S(1) H(28) 3.2553 ? . . S(1) H(31) 3.0373 ? . 45501 S(1) H(32) 3.1111 ? . 45501 S(2) H(5) 3.1631 ? . 54503 S(2) H(6) 3.0787 ? . 54503 S(2) H(13) 3.2038 ? . 45501 S(2) H(22) 3.4537 ? . 45501 S(2) H(23) 3.3798 ? . 45501 S(3) H(1) 3.1329 ? . . S(3) H(5) 2.9586 ? . 54503 S(3) H(7) 2.9912 ? . 45501 S(3) H(11) 2.9349 ? . . S(3) H(12) 3.5934 ? . 45501 S(3) H(13) 3.2612 ? . 45501 S(3) H(20) 3.5459 ? . . S(3) H(21) 3.1032 ? . . S(4) H(27) 3.5103 ? . 45602 S(4) H(30) 3.0025 ? . 45602 S(4) H(32) 2.9728 ? . 45501 S(4) H(33) 3.3772 ? . 45501 S(4) H(34) 3.5159 ? . . O(1) H(1) 1.9210 ? . . O(1) H(2) 2.3379 ? . . O(1) H(7) 3.3188 ? . . O(1) H(11) 3.0732 ? . . O(1) H(13) 3.0060 ? . . O(1) H(14) 3.0479 ? . . O(1) H(22) 2.6668 ? . . O(1) H(26) 3.5568 ? . . O(1) H(33) 2.6246 ? . . O(1) H(34) 3.2051 ? . . N(1) H(7) 2.0175 ? . . N(1) H(8) 2.0216 ? . . N(1) H(9) 2.8898 ? . . N(1) H(10) 3.2586 ? . . N(1) H(11) 2.4793 ? . . N(1) H(12) 2.0200 ? . . N(1) H(13) 2.0243 ? . . N(1) H(14) 2.9334 ? . . N(1) H(15) 3.2819 ? . . N(1) H(16) 2.5295 ? . . N(1) H(17) 2.9527 ? . . N(1) H(18) 3.2943 ? . . N(1) H(19) 2.5471 ? . . N(1) H(20) 2.0110 ? . . N(1) H(21) 2.0275 ? . . N(2) H(22) 2.0181 ? . . N(2) H(23) 2.0255 ? . . N(2) H(24) 2.9401 ? . . N(2) H(25) 3.2883 ? . . N(2) H(26) 2.5467 ? . . N(2) H(27) 2.0024 ? . . N(2) H(28) 2.0197 ? . . N(2) H(29) 2.8969 ? . . N(2) H(30) 3.2624 ? . . N(2) H(31) 2.5111 ? . . N(2) H(32) 2.0424 ? . . N(2) H(33) 2.0402 ? . . N(2) H(34) 2.9346 ? . . N(2) H(35) 3.2883 ? . . N(2) H(36) 2.5125 ? . . C(1) H(2) 3.5992 ? . . C(1) H(4) 3.3139 ? . . C(1) H(23) 2.6364 ? . 45501 C(1) H(26) 2.7211 ? . . C(1) H(31) 3.3670 ? . 45501 C(2) H(3) 3.2945 ? . . C(2) H(22) 3.4886 ? . 45501 C(2) H(23) 2.7451 ? . 45501 C(2) H(26) 3.2220 ? . . C(3) H(3) 2.0217 ? . . C(3) H(4) 3.2612 ? . . C(3) H(23) 3.3044 ? . 45501 C(3) H(25) 3.4647 ? . 45501 C(3) H(25) 3.5797 ? . 44602 C(4) H(4) 2.0505 ? . . C(4) H(24) 3.5020 ? . 45501 C(4) H(25) 3.2571 ? . 44602 C(5) H(3) 2.0413 ? . . C(5) H(9) 3.2039 ? . 55504 C(6) H(3) 3.2582 ? . . C(6) H(4) 2.0590 ? . . C(6) H(23) 3.2017 ? . 45501 C(6) H(26) 3.1045 ? . . C(6) H(29) 3.2420 ? . 45501 C(6) H(31) 3.4350 ? . 45501 C(7) H(6) 3.3055 ? . . C(7) H(7) 2.9249 ? . 45501 C(7) H(11) 3.0732 ? . . C(8) H(5) 3.2970 ? . . C(8) H(19) 3.2297 ? . 65503 C(9) H(5) 2.0458 ? . . C(9) H(6) 3.2838 ? . . C(9) H(12) 3.0957 ? . 65503 C(9) H(19) 2.9074 ? . 65503 C(9) H(20) 3.5624 ? . 55503 C(10) H(6) 2.0706 ? . . C(10) H(12) 2.6433 ? . 65503 C(10) H(15) 3.5304 ? . 65503 C(10) H(19) 3.3639 ? . 65503 C(10) H(20) 2.8432 ? . 55503 C(10) H(21) 3.4644 ? . 55503 C(11) H(5) 2.0599 ? . . C(11) H(10) 3.3758 ? . 45501 C(11) H(12) 3.2472 ? . 65503 C(11) H(15) 3.1727 ? . 65503 C(11) H(20) 3.5183 ? . 55503 C(12) H(5) 3.2541 ? . . C(12) H(6) 2.0427 ? . . C(12) H(7) 3.1229 ? . 45501 C(12) H(8) 3.4314 ? . 45501 C(12) H(10) 3.3767 ? . 45501 C(12) H(11) 3.5458 ? . . C(13) H(1) 1.9895 ? . . C(13) H(9) 2.0018 ? . . C(13) H(10) 2.0301 ? . . C(13) H(11) 1.9964 ? . . C(13) H(12) 2.6305 ? . . C(13) H(13) 2.5691 ? . . C(13) H(17) 3.1538 ? . . C(13) H(19) 3.1273 ? . . C(13) H(20) 3.3224 ? . . C(13) H(21) 2.6942 ? . . C(14) H(1) 2.5737 ? . . C(14) H(4) 3.1629 ? . 55404 C(14) H(7) 1.9883 ? . . C(14) H(8) 2.0015 ? . . C(14) H(21) 2.7921 ? . . C(15) H(1) 1.9905 ? . . C(15) H(5) 3.3222 ? . 64503 C(15) H(7) 2.4968 ? . . C(15) H(8) 2.7228 ? . . C(15) H(14) 2.0433 ? . . C(15) H(15) 2.0476 ? . . C(15) H(16) 2.0364 ? . . C(15) H(19) 2.5783 ? . . C(15) H(20) 2.6949 ? . . C(15) H(21) 3.3201 ? . . C(15) H(22) 3.2001 ? . . C(16) H(1) 2.6736 ? . . C(16) H(3) 3.3893 ? . 54602 C(16) H(12) 2.0334 ? . . C(16) H(13) 2.0320 ? . . C(16) H(19) 3.1730 ? . . C(16) H(20) 2.6412 ? . . C(16) H(22) 3.1573 ? . . C(16) H(25) 3.3810 ? . . C(17) H(1) 2.0033 ? . . C(17) H(5) 3.0381 ? . 54503 C(17) H(7) 3.3336 ? . . C(17) H(8) 2.6912 ? . . C(17) H(9) 3.0849 ? . . C(17) H(11) 3.0722 ? . . C(17) H(12) 2.7290 ? . . C(17) H(13) 3.3171 ? . . C(17) H(14) 3.5856 ? . . C(17) H(16) 2.5052 ? . . C(17) H(17) 2.0336 ? . . C(17) H(18) 2.0450 ? . . C(17) H(19) 2.0264 ? . . C(18) H(1) 3.3191 ? . . C(18) H(8) 2.8290 ? . . C(18) H(12) 2.7422 ? . . C(18) H(16) 3.1278 ? . . C(18) H(20) 2.0176 ? . . C(18) H(21) 2.0202 ? . . C(18) H(30) 3.5495 ? . 65404 C(18) H(34) 3.3505 ? . 64503 C(19) H(2) 2.0004 ? . . C(19) H(13) 3.4596 ? . . C(19) H(14) 3.1612 ? . . C(19) H(24) 2.0406 ? . . C(19) H(25) 2.0501 ? . . C(19) H(26) 2.0461 ? . . C(19) H(27) 3.3151 ? . . C(19) H(28) 2.7639 ? . . C(19) H(29) 2.9775 ? . . C(19) H(31) 2.8890 ? . . C(19) H(32) 2.6707 ? . . C(19) H(33) 2.5485 ? . . C(20) H(2) 2.6766 ? . . C(20) H(3) 3.4760 ? . 54602 C(20) H(14) 3.1093 ? . . C(20) H(22) 2.0314 ? . . C(20) H(23) 2.0402 ? . . C(20) H(28) 2.7689 ? . . C(20) H(29) 3.2162 ? . . C(21) H(2) 1.9860 ? . . C(21) H(22) 3.3144 ? . . C(21) H(23) 2.7334 ? . . C(21) H(24) 3.0243 ? . . C(21) H(26) 2.9534 ? . . C(21) H(29) 2.0054 ? . . C(21) H(30) 2.0468 ? . . C(21) H(31) 2.0347 ? . . C(21) H(32) 2.7402 ? . . C(21) H(33) 3.3352 ? . . C(21) H(36) 2.5869 ? . . C(22) H(2) 3.2827 ? . . C(22) H(17) 3.3610 ? . 65504 C(22) H(23) 2.6980 ? . . C(22) H(24) 3.2431 ? . . C(22) H(27) 1.9972 ? . . C(22) H(28) 2.0382 ? . . C(22) H(32) 2.8347 ? . . C(22) H(34) 3.5375 ? . 55602 C(22) H(36) 3.4418 ? . . C(22) H(36) 3.3267 ? . 55602 C(23) H(2) 2.0112 ? . . C(23) H(22) 2.5466 ? . . C(23) H(23) 2.6469 ? . . C(23) H(27) 2.6435 ? . . C(23) H(28) 3.3390 ? . . C(23) H(31) 2.7240 ? . . C(23) H(34) 2.0479 ? . . C(23) H(35) 2.0445 ? . . C(23) H(36) 2.0231 ? . . C(24) H(2) 2.6470 ? . . C(24) H(18) 3.4929 ? . 65503 C(24) H(27) 2.6494 ? . . C(24) H(30) 3.3229 ? . 45602 C(24) H(31) 3.5586 ? . . C(24) H(31) 3.3874 ? . 45602 C(24) H(32) 2.0375 ? . . C(24) H(33) 2.0212 ? . . H(3) C(6) 3.2582 ? . . H(3) C(16) 3.3893 ? . 44602 H(3) C(20) 3.4760 ? . 44602 H(4) C(6) 2.0590 ? . . H(4) C(14) 3.1629 ? . 55504 H(5) S(2) 3.1631 ? . 55503 H(5) S(3) 2.9586 ? . 55503 H(5) C(15) 3.3222 ? . 65503 H(5) C(17) 3.0381 ? . 55503 H(6) Cl(2) 2.7924 ? . 55503 H(6) S(2) 3.0787 ? . 55503 H(7) Cl(3) 3.5201 ? . 65501 H(7) S(3) 2.9912 ? . 65501 H(7) C(7) 2.9249 ? . 65501 H(7) C(12) 3.1229 ? . 65501 H(8) Cl(3) 3.0344 ? . 65501 H(8) Cl(4) 3.5688 ? . 64503 H(8) C(12) 3.4314 ? . 65501 H(9) Cl(1) 3.4205 ? . 55404 H(9) C(5) 3.2039 ? . 55404 H(10) C(11) 3.3758 ? . 65501 H(10) C(12) 3.3767 ? . 65501 H(12) S(3) 3.5934 ? . 65501 H(12) C(9) 3.0957 ? . 64503 H(12) C(10) 2.6433 ? . 64503 H(12) C(11) 3.2472 ? . 64503 H(13) S(2) 3.2038 ? . 65501 H(13) S(3) 3.2612 ? . 65501 H(15) Cl(2) 3.3989 ? . 65501 H(15) C(10) 3.5304 ? . 64503 H(15) C(11) 3.1727 ? . 64503 H(17) Cl(1) 3.0122 ? . 55404 H(17) C(22) 3.3610 ? . 65404 H(18) C(24) 3.4929 ? . 64503 H(19) Cl(4) 3.2078 ? . 64503 H(19) C(8) 3.2297 ? . 64503 H(19) C(9) 2.9074 ? . 64503 H(19) C(10) 3.3639 ? . 64503 H(20) C(9) 3.5624 ? . 54503 H(20) C(10) 2.8432 ? . 54503 H(20) C(11) 3.5183 ? . 54503 H(21) Cl(1) 3.3853 ? . 55404 H(21) Cl(4) 3.3126 ? . 54503 H(21) C(10) 3.4644 ? . 54503 H(22) S(2) 3.4537 ? . 65501 H(22) C(2) 3.4886 ? . 65501 H(23) S(1) 3.1019 ? . 65501 H(23) S(2) 3.3798 ? . 65501 H(23) N(2) 2.0255 ? . . H(23) C(1) 2.6364 ? . 65501 H(23) C(2) 2.7451 ? . 65501 H(23) C(3) 3.3044 ? . 65501 H(23) C(6) 3.2017 ? . 65501 H(23) C(20) 2.0402 ? . . H(23) C(21) 2.7334 ? . . H(23) C(22) 2.6980 ? . . H(23) C(23) 2.6469 ? . . H(24) Cl(2) 3.2123 ? . 54602 H(24) C(4) 3.5020 ? . 65501 H(25) Cl(2) 3.1417 ? . 54602 H(25) C(3) 3.4647 ? . 65501 H(25) C(3) 3.5797 ? . 54602 H(25) C(4) 3.2571 ? . 54602 H(26) Cl(2) 3.5326 ? . 54602 H(26) C(6) 3.1045 ? . . H(27) S(4) 3.5103 ? . 55602 H(28) Cl(4) 3.2620 ? . 55602 H(29) Cl(1) 3.2261 ? . 65501 H(29) Cl(4) 3.5570 ? . 55602 H(29) C(6) 3.2420 ? . 65501 H(30) Cl(4) 3.2289 ? . 55602 H(30) S(4) 3.0025 ? . 55602 H(30) C(18) 3.5495 ? . 65504 H(30) C(24) 3.3229 ? . 55602 H(31) Cl(1) 3.3260 ? . 65501 H(31) S(1) 3.0373 ? . 65501 H(31) C(1) 3.3670 ? . 65501 H(31) C(6) 3.4350 ? . 65501 H(31) C(24) 3.3874 ? . 55602 H(32) S(1) 3.1111 ? . 65501 H(32) S(4) 2.9728 ? . 65501 H(33) S(4) 3.3772 ? . 65501 H(34) C(18) 3.3505 ? . 65503 H(34) C(22) 3.5375 ? . 45602 H(35) Cl(1) 3.1665 ? . 55602 H(35) Cl(4) 3.3840 ? . 65501 H(36) C(22) 3.3267 ? . 45602 O(1) N(1) 2.809(7) ? . . O(1) N(2) 2.979(6) ? . . #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #============================================================================== data_(Et4N)[3] _database_code_depnum_ccdc_archive 'CCDC 253878' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C20 H24 Cl4 N Mo O S4 ' _chemical_formula_moiety 'C20 H24 Cl4 N Mo O S4 ' _chemical_formula_weight 660.41 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 c 1' _symmetry_space_group_name_Hall 'P -2yc' _symmetry_Int_Tables_number 7 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 +X,-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 9.269(3) _cell_length_b 8.222(2) _cell_length_c 17.337(5) _cell_angle_alpha 90 _cell_angle_beta 103.143(6) _cell_angle_gamma 90 _cell_volume 1286.7(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4236 _cell_measurement_theta_min 4.4 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 173.1 #------------------------------------------------------------------------------ _exptl_crystal_description platelet _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 666.00 _exptl_absorpt_coefficient_mu 1.263 _exptl_absorpt_correction_type none #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 6240 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9895 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9895 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 2927 _reflns_number_gt 2262 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.0980 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 2927 _refine_ls_number_parameters 317 _refine_ls_goodness_of_fit_ref 0.974 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0003Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.89 _refine_diff_density_min -0.67 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mo Mo -1.683 0.686 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo(1) Mo 0.4348(2) 0.0753(2) 0.26464(12) 0.0173(3) Uani 0.65 1 d P . . Mo(2) Mo 0.5236(3) -0.0742(4) 0.3027(2) 0.0247(7) Uani 0.35 1 d P . . Cl(1) Cl 0.1860(4) -0.0254(4) 0.5180(2) 0.0340(8) Uani 1.00 1 d . . . Cl(2) Cl -0.0395(5) -0.3163(4) 0.1805(2) 0.0414(10) Uani 1.00 1 d . . . Cl(3) Cl 0.7675(4) 0.0252(4) 0.0493(2) 0.0347(8) Uani 1.00 1 d . . . Cl(4) Cl 0.9905(4) 0.3095(5) 0.3875(2) 0.0413(10) Uani 1.00 1 d . . . S(1) S 0.3797(4) 0.0250(4) 0.3917(2) 0.0305(8) Uani 1.00 1 d . . . S(2) S 0.2676(4) -0.1325(4) 0.2194(2) 0.0317(9) Uani 1.00 1 d . . . S(3) S 0.5701(4) -0.0238(4) 0.1750(2) 0.0308(8) Uani 1.00 1 d . . . S(4) S 0.6803(4) 0.1278(4) 0.3468(2) 0.0325(9) Uani 1.00 1 d . . . O(1) O 0.3598(13) 0.252(1) 0.2315(6) 0.024(3) Uani 0.65 1 d P . . O(2) O 0.601(3) -0.264(3) 0.339(2) 0.046(8) Uani 0.35 1 d P . . N(1) N 0.474(1) 0.4889(6) 0.5351(7) 0.025(1) Uani 1.00 1 d . . . C(1) C 0.2105(11) -0.089(2) 0.3673(6) 0.022(3) Uani 1.00 1 d . . . C(2) C 0.1608(12) -0.1490(13) 0.2906(7) 0.023(3) Uani 1.00 1 d . . . C(3) C 0.0269(12) -0.234(1) 0.2727(7) 0.026(3) Uani 1.00 1 d . . . C(4) C -0.0646(13) -0.241(2) 0.3297(7) 0.033(3) Uani 1.00 1 d . . . C(5) C -0.014(2) -0.183(2) 0.4025(9) 0.035(4) Uani 1.00 1 d . . . C(6) C 0.1251(12) -0.102(1) 0.4232(6) 0.023(3) Uani 1.00 1 d . . . C(7) C 0.7398(11) 0.071(1) 0.2004(6) 0.021(2) Uani 1.00 1 d . . . C(8) C 0.7906(12) 0.1445(13) 0.2763(7) 0.024(3) Uani 1.00 1 d . . . C(9) C 0.926(2) 0.222(1) 0.2939(7) 0.031(3) Uani 1.00 1 d . . . C(10) C 1.006(1) 0.249(2) 0.2394(8) 0.034(4) Uani 1.00 1 d . . . C(11) C 0.959(1) 0.177(2) 0.1629(7) 0.030(3) Uani 1.00 1 d . . . C(12) C 0.830(1) 0.098(2) 0.1457(6) 0.027(3) Uani 1.00 1 d . . . C(13) C 0.603(1) 0.3799(13) 0.5242(7) 0.031(3) Uani 1.00 1 d . . . C(14) C 0.7390(12) 0.466(2) 0.5094(8) 0.040(4) Uani 1.00 1 d . . . C(15) C 0.3498(13) 0.377(2) 0.5422(7) 0.035(4) Uani 1.00 1 d . . . C(16) C 0.218(2) 0.467(2) 0.5587(8) 0.054(5) Uani 1.00 1 d . . . C(17) C 0.435(2) 0.601(2) 0.4624(7) 0.048(3) Uani 1.00 1 d . . . C(18) C 0.391(2) 0.520(2) 0.3839(7) 0.049(4) Uani 1.00 1 d . . . C(19) C 0.528(1) 0.598(2) 0.6058(7) 0.038(3) Uiso 1.00 1 d . . . C(20) C 0.573(2) 0.499(2) 0.6846(7) 0.049(4) Uani 1.00 1 d . . . H(1) H -0.1578 -0.2946 0.3156 0.038 Uiso 1.00 1 c R . . H(2) H -0.0700 -0.1911 0.4420 0.043 Uiso 1.00 1 c R . . H(3) H 1.0957 0.3093 0.2518 0.043 Uiso 1.00 1 c R . . H(4) H 1.0176 0.1869 0.1248 0.037 Uiso 1.00 1 c R . . H(5) H 0.6317 0.3089 0.5683 0.037 Uiso 1.00 1 c R . . H(6) H 0.5646 0.3179 0.4779 0.037 Uiso 1.00 1 c R . . H(7) H 0.7287 0.4899 0.4548 0.050 Uiso 1.00 1 c R . . H(8) H 0.8245 0.4002 0.5274 0.050 Uiso 1.00 1 c R . . H(9) H 0.7491 0.5640 0.5389 0.050 Uiso 1.00 1 c R . . H(10) H 0.3169 0.3274 0.4918 0.041 Uiso 1.00 1 c R . . H(11) H 0.3826 0.2959 0.5811 0.041 Uiso 1.00 1 c R . . H(12) H 0.2290 0.4673 0.6145 0.061 Uiso 1.00 1 c R . . H(13) H 0.1286 0.4134 0.5343 0.061 Uiso 1.00 1 c R . . H(14) H 0.2155 0.5758 0.5400 0.061 Uiso 1.00 1 c R . . H(15) H 0.3655 0.6805 0.4699 0.063 Uiso 1.00 1 c R . . H(16) H 0.5253 0.6523 0.4591 0.063 Uiso 1.00 1 c R . . H(17) H 0.4707 0.4856 0.3616 0.059 Uiso 1.00 1 c R . . H(18) H 0.3286 0.5914 0.3479 0.059 Uiso 1.00 1 c R . . H(19) H 0.3361 0.4286 0.3938 0.059 Uiso 1.00 1 c R . . H(20) H 0.6157 0.6504 0.6001 0.046 Uiso 1.00 1 c R . . H(21) H 0.4540 0.6769 0.6081 0.045 Uiso 1.00 1 c R . . H(22) H 0.4866 0.4934 0.7051 0.057 Uiso 1.00 1 c R . . H(23) H 0.6509 0.5486 0.7227 0.057 Uiso 1.00 1 c R . . H(24) H 0.6023 0.3924 0.6735 0.057 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mo(1) 0.0179(6) 0.0189(6) 0.0162(6) 0.0010(7) 0.0058(5) 0.0095(7) Mo(2) 0.025(2) 0.028(1) 0.0246(13) -0.003(1) 0.0140(12) -0.012(1) Cl(1) 0.037(2) 0.046(2) 0.0208(13) -0.006(1) 0.0101(13) -0.0040(13) Cl(2) 0.045(2) 0.045(2) 0.032(2) -0.008(2) 0.004(2) -0.013(2) Cl(3) 0.042(2) 0.043(2) 0.022(1) -0.003(1) 0.015(1) -0.0025(13) Cl(4) 0.030(2) 0.061(2) 0.031(2) 0.001(2) 0.003(1) -0.014(2) S(1) 0.038(2) 0.034(2) 0.023(2) -0.0063(13) 0.014(1) -0.0062(13) S(2) 0.035(2) 0.043(2) 0.021(2) -0.004(1) 0.0138(13) 0.0007(12) S(3) 0.029(2) 0.041(2) 0.026(2) -0.0089(13) 0.013(1) -0.0050(13) S(4) 0.036(2) 0.042(2) 0.021(2) 0.003(1) 0.0089(13) -0.0067(13) O(1) 0.031(6) 0.014(5) 0.024(6) 0.013(5) 0.001(5) 0.012(5) O(2) 0.03(1) 0.05(2) 0.06(2) -0.014(12) 0.023(13) 0.001(13) N(1) 0.037(3) 0.019(3) 0.022(3) 0.016(5) 0.012(2) 0.012(5) C(1) 0.021(5) 0.016(5) 0.030(6) -0.000(4) 0.008(4) 0.002(4) C(2) 0.022(6) 0.028(6) 0.022(6) 0.000(5) 0.012(5) 0.002(4) C(3) 0.016(5) 0.029(6) 0.032(7) -0.007(5) 0.005(5) 0.002(5) C(4) 0.015(5) 0.045(8) 0.034(7) 0.015(5) -0.006(5) 0.006(6) C(5) 0.035(7) 0.030(7) 0.044(8) -0.001(5) 0.016(6) 0.001(6) C(6) 0.026(6) 0.021(6) 0.021(6) 0.004(5) 0.005(4) 0.004(5) C(7) 0.031(5) 0.011(4) 0.022(5) 0.004(4) 0.008(4) 0.001(4) C(8) 0.024(6) 0.020(5) 0.028(6) 0.011(5) 0.004(5) -0.000(5) C(9) 0.048(8) 0.026(6) 0.015(5) 0.024(5) -0.004(5) -0.008(4) C(10) 0.035(7) 0.028(6) 0.043(8) -0.012(5) 0.016(6) -0.015(6) C(11) 0.026(6) 0.051(8) 0.016(6) 0.006(5) 0.013(5) 0.000(5) C(12) 0.036(7) 0.027(7) 0.021(6) 0.004(5) 0.014(5) -0.004(5) C(13) 0.048(8) 0.017(6) 0.028(6) 0.007(5) 0.007(6) -0.003(5) C(14) 0.025(6) 0.055(9) 0.046(8) -0.003(6) 0.021(6) -0.003(6) C(15) 0.027(6) 0.046(8) 0.030(7) -0.005(5) 0.002(5) -0.006(6) C(16) 0.051(8) 0.064(11) 0.039(8) -0.002(8) -0.009(7) -0.011(7) C(17) 0.090(9) 0.030(6) 0.038(6) 0.037(6) 0.041(6) 0.025(4) C(18) 0.054(8) 0.062(9) 0.032(6) 0.042(7) 0.013(6) 0.015(6) C(20) 0.078(10) 0.043(7) 0.022(6) 0.014(7) 0.003(7) -0.011(5) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution ? _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mo(1) Mo(2) 1.541(4) ? . . Mo(1) S(1) 2.407(4) ? . . Mo(1) S(2) 2.320(4) ? . . Mo(1) S(3) 2.353(4) ? . . Mo(1) S(4) 2.433(4) ? . . Mo(1) O(1) 1.66(1) ? . . Mo(2) S(1) 2.400(5) ? . . Mo(2) S(2) 2.527(4) ? . . Mo(2) S(3) 2.385(5) ? . . Mo(2) S(4) 2.224(5) ? . . Mo(2) O(2) 1.77(3) ? . . Cl(1) C(6) 1.73(1) ? . . Cl(2) C(3) 1.72(1) ? . . Cl(3) C(12) 1.75(1) ? . . Cl(4) C(9) 1.75(1) ? . . S(1) C(1) 1.79(1) ? . . S(2) C(2) 1.75(1) ? . . S(3) C(7) 1.72(1) ? . . S(4) C(8) 1.77(1) ? . . O(1) Mo(1) 1.66(1) ? . . N(1) C(13) 1.54(2) ? . . N(1) C(15) 1.50(2) ? . . N(1) C(17) 1.54(2) ? . . N(1) C(19) 1.51(2) ? . . C(1) C(2) 1.39(2) ? . . C(1) C(6) 1.39(2) ? . . C(2) C(3) 1.40(2) ? . . C(3) C(4) 1.44(2) ? . . C(4) C(5) 1.33(2) ? . . C(5) C(6) 1.42(2) ? . . C(7) S(3) 1.72(1) ? . . C(7) C(8) 1.43(1) ? . . C(7) C(12) 1.42(2) ? . . C(8) C(7) 1.43(1) ? . . C(8) C(9) 1.38(2) ? . . C(9) C(10) 1.35(2) ? . . C(10) C(11) 1.42(2) ? . . C(11) C(12) 1.33(2) ? . . C(12) C(7) 1.42(2) ? . . C(13) C(14) 1.51(2) ? . . C(15) C(16) 1.51(2) ? . . C(17) C(18) 1.48(2) ? . . C(19) C(20) 1.56(2) ? . . C(4) H(1) 0.9500 ? . . C(5) H(2) 0.9500 ? . . C(10) H(3) 0.9500 ? . . C(11) H(4) 0.9500 ? . . C(13) H(5) 0.9500 ? . . C(13) H(6) 0.9501 ? . . C(14) H(7) 0.9500 ? . . C(14) H(8) 0.9500 ? . . C(14) H(9) 0.9500 ? . . C(15) H(10) 0.9499 ? . . C(15) H(11) 0.9500 ? . . C(16) H(12) 0.9500 ? . . C(16) H(13) 0.9500 ? . . C(16) H(14) 0.9501 ? . . C(17) H(15) 0.9500 ? . . C(17) H(16) 0.9500 ? . . C(18) H(17) 0.9500 ? . . C(18) H(18) 0.9500 ? . . C(18) H(19) 0.9500 ? . . C(19) H(20) 0.9500 ? . . C(19) H(21) 0.9500 ? . . C(20) H(22) 0.9500 ? . . C(20) H(23) 0.9500 ? . . C(20) H(24) 0.9500 ? . . H(4) C(11) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Mo(1) Mo(2) S(1) 71.5(2) ? . . . S(1) Mo(1) Mo(2) 71.1(2) ? . . . Mo(1) Mo(2) S(2) 64.3(1) ? . . . S(2) Mo(1) Mo(2) 78.9(2) ? . . . Mo(1) Mo(2) S(3) 69.9(2) ? . . . S(3) Mo(1) Mo(2) 72.2(2) ? . . . Mo(1) Mo(2) S(4) 78.2(2) ? . . . S(4) Mo(1) Mo(2) 63.5(2) ? . . . O(1) Mo(1) Mo(2) 171.6(4) ? . . . Mo(1) Mo(2) O(2) 171.0(8) ? . . . Mo(1) S(1) Mo(2) 37.4(1) ? . . . S(2) Mo(1) S(1) 85.3(1) ? . . . S(3) Mo(1) S(1) 143.2(1) ? . . . S(4) Mo(1) S(1) 81.9(1) ? . . . O(1) Mo(1) S(1) 108.0(4) ? . . . Mo(1) S(1) C(1) 103.3(4) ? . . . Mo(1) S(2) Mo(2) 36.8(1) ? . . . S(3) Mo(1) S(2) 86.4(1) ? . . . S(4) Mo(1) S(2) 142.4(1) ? . . . O(1) Mo(1) S(2) 109.4(4) ? . . . Mo(1) S(2) C(2) 105.0(4) ? . . . Mo(1) S(3) Mo(2) 38.0(1) ? . . . S(4) Mo(1) S(3) 83.1(1) ? . . . O(1) Mo(1) S(3) 108.6(4) ? . . . Mo(1) S(3) C(7) 105.6(4) ? . . . Mo(1) S(4) Mo(2) 38.3(1) ? . . . O(1) Mo(1) S(4) 108.1(4) ? . . . Mo(1) S(4) C(8) 102.7(4) ? . . . S(2) Mo(2) S(1) 81.1(1) ? . . . S(3) Mo(2) S(1) 141.4(2) ? . . . S(4) Mo(2) S(1) 86.5(2) ? . . . O(2) Mo(2) S(1) 107.9(9) ? . . . Mo(2) S(1) C(1) 104.7(4) ? . . . S(3) Mo(2) S(2) 81.2(1) ? . . . S(4) Mo(2) S(2) 142.5(2) ? . . . O(2) Mo(2) S(2) 106.7(8) ? . . . Mo(2) S(2) C(2) 102.7(4) ? . . . S(4) Mo(2) S(3) 87.0(2) ? . . . O(2) Mo(2) S(3) 110.0(9) ? . . . Mo(2) S(3) C(7) 100.9(4) ? . . . O(2) Mo(2) S(4) 110.8(8) ? . . . Mo(2) S(4) C(8) 104.8(4) ? . . . Cl(1) C(6) C(1) 121.4(8) ? . . . Cl(1) C(6) C(5) 119(1) ? . . . Cl(2) C(3) C(2) 121(1) ? . . . Cl(2) C(3) C(4) 118.6(8) ? . . . Cl(3) C(12) C(7) 117.9(9) ? . . . Cl(3) C(12) C(11) 117(1) ? . . . Cl(4) C(9) C(8) 119(1) ? . . . Cl(4) C(9) C(10) 117(1) ? . . . S(1) C(1) C(6) 118.8(8) ? . . . S(1) C(1) C(2) 119.4(9) ? . . . S(2) C(2) C(1) 121.8(9) ? . . . S(2) C(2) C(3) 119.8(9) ? . . . S(3) C(7) C(12) 123.0(8) ? . . . S(3) C(7) C(8) 121.2(9) ? . . . S(4) C(8) C(7) 118.8(8) ? . . . S(4) C(8) C(9) 121.5(9) ? . . . N(1) C(13) C(14) 116.7(9) ? . . . C(15) N(1) C(13) 106.7(7) ? . . . C(17) N(1) C(13) 106(1) ? . . . C(19) N(1) C(13) 108(1) ? . . . N(1) C(15) C(16) 112(1) ? . . . C(17) N(1) C(15) 113(1) ? . . . C(19) N(1) C(15) 114(1) ? . . . N(1) C(17) C(18) 116(1) ? . . . C(19) N(1) C(17) 106.6(7) ? . . . N(1) C(19) C(20) 112(1) ? . . . C(6) C(1) C(2) 121(1) ? . . . C(1) C(2) C(3) 118(1) ? . . . C(1) C(6) C(5) 119(1) ? . . . C(2) C(3) C(4) 119(1) ? . . . C(3) C(4) C(5) 119(1) ? . . . C(4) C(5) C(6) 120(1) ? . . . C(12) C(7) C(8) 115(1) ? . . . C(7) C(8) C(9) 119(1) ? . . . C(7) C(12) C(11) 124(1) ? . . . C(8) C(9) C(10) 122(1) ? . . . C(9) C(10) C(11) 118(1) ? . . . C(10) C(11) C(12) 118(1) ? . . . N(1) C(13) H(5) 109.7791 ? . . . N(1) C(13) H(6) 105.0607 ? . . . N(1) C(15) H(10) 106.3377 ? . . . N(1) C(15) H(11) 111.2476 ? . . . N(1) C(17) H(15) 109.8886 ? . . . N(1) C(17) H(16) 105.7756 ? . . . N(1) C(19) H(20) 108.5849 ? . . . N(1) C(19) H(21) 109.5150 ? . . . C(3) C(4) H(1) 119.0368 ? . . . C(4) C(5) H(2) 121.7795 ? . . . H(1) C(4) C(5) 120.8328 ? . . . H(2) C(5) C(6) 117.5909 ? . . . C(9) C(10) H(3) 121.1964 ? . . . C(10) C(11) H(4) 120.5219 ? . . . H(3) C(10) C(11) 119.7766 ? . . . H(4) C(11) C(12) 120.8265 ? . . . H(5) C(13) C(14) 109.5601 ? . . . H(6) C(13) C(14) 105.9574 ? . . . C(13) C(14) H(7) 111.5560 ? . . . C(13) C(14) H(9) 106.7746 ? . . . C(13) C(14) H(8) 110.0379 ? . . . H(6) C(13) H(5) 109.4616 ? . . . H(9) C(14) H(7) 109.4746 ? . . . H(8) C(14) H(7) 109.4752 ? . . . H(9) C(14) H(8) 109.4711 ? . . . H(10) C(15) C(16) 106.2874 ? . . . H(11) C(15) C(16) 110.6029 ? . . . C(15) C(16) H(12) 106.9640 ? . . . C(15) C(16) H(14) 110.8171 ? . . . C(15) C(16) H(13) 110.5969 ? . . . H(11) C(15) H(10) 109.4592 ? . . . H(14) C(16) H(12) 109.4739 ? . . . H(13) C(16) H(12) 109.4755 ? . . . H(14) C(16) H(13) 109.4702 ? . . . C(17) C(18) H(17) 115.5470 ? . . . H(15) C(17) C(18) 112.2997 ? . . . H(16) C(17) C(18) 101.8623 ? . . . C(17) C(18) H(19) 103.4598 ? . . . C(17) C(18) H(18) 109.1774 ? . . . H(16) C(17) H(15) 109.4599 ? . . . H(19) C(18) H(17) 109.4726 ? . . . H(18) C(18) H(17) 109.4712 ? . . . H(19) C(18) H(18) 109.4747 ? . . . H(20) C(19) C(20) 105.0321 ? . . . H(21) C(19) C(20) 111.9332 ? . . . C(19) C(20) H(22) 105.4481 ? . . . C(19) C(20) H(24) 109.4980 ? . . . C(19) C(20) H(23) 113.3655 ? . . . H(21) C(19) H(20) 109.4556 ? . . . H(24) C(20) H(22) 109.4726 ? . . . H(23) C(20) H(22) 109.4683 ? . . . H(24) C(20) H(23) 109.4774 ? . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 S(1) Mo(1) Mo(2) S(2) 88.8(1) ? . . . . S(1) Mo(1) Mo(2) S(3) 178.6(1) ? . . . . S(1) Mo(1) Mo(2) S(4) -90.3(1) ? . . . . S(2) Mo(1) Mo(2) S(1) -88.8(1) ? . . . . S(2) Mo(1) Mo(2) S(3) 89.7(1) ? . . . . S(2) Mo(1) Mo(2) S(4) -179.1(2) ? . . . . S(3) Mo(1) Mo(2) S(1) -178.6(1) ? . . . . S(3) Mo(1) Mo(2) S(2) -89.7(1) ? . . . . S(3) Mo(1) Mo(2) S(4) 91.2(1) ? . . . . S(4) Mo(1) Mo(2) S(1) 90.3(1) ? . . . . S(4) Mo(1) Mo(2) S(2) 179.1(2) ? . . . . S(4) Mo(1) Mo(2) S(3) -91.2(1) ? . . . . Mo(2) Mo(1) S(1) C(1) -96.9(4) ? . . . . S(2) Mo(1) S(1) Mo(2) 79.9(1) ? . . . . S(2) Mo(1) S(1) C(1) -17.0(4) ? . . . . S(3) Mo(1) S(1) Mo(2) 2.3(2) ? . . . . S(3) Mo(1) S(1) C(1) -94.6(4) ? . . . . S(4) Mo(1) S(1) Mo(2) -64.7(1) ? . . . . S(4) Mo(1) S(1) C(1) -161.6(4) ? . . . . O(1) Mo(1) S(1) Mo(2) -171.2(2) ? . . . . O(1) Mo(1) S(1) C(1) 91.9(4) ? . . . . Mo(2) Mo(1) S(2) C(2) 91.1(4) ? . . . . S(1) Mo(1) S(2) Mo(2) -71.6(2) ? . . . . S(1) Mo(1) S(2) C(2) 19.6(4) ? . . . . S(3) Mo(1) S(2) Mo(2) 72.5(2) ? . . . . S(3) Mo(1) S(2) C(2) 163.7(4) ? . . . . S(4) Mo(1) S(2) Mo(2) -1.3(2) ? . . . . S(4) Mo(1) S(2) C(2) 89.8(4) ? . . . . O(1) Mo(1) S(2) Mo(2) -179.0(2) ? . . . . O(1) Mo(1) S(2) C(2) -87.9(4) ? . . . . Mo(2) Mo(1) S(3) C(7) -87.8(4) ? . . . . S(1) Mo(1) S(3) Mo(2) -2.3(2) ? . . . . S(1) Mo(1) S(3) C(7) -90.1(4) ? . . . . S(2) Mo(1) S(3) Mo(2) -79.5(1) ? . . . . S(2) Mo(1) S(3) C(7) -167.3(4) ? . . . . S(4) Mo(1) S(3) Mo(2) 64.3(1) ? . . . . S(4) Mo(1) S(3) C(7) -23.5(4) ? . . . . O(1) Mo(1) S(3) Mo(2) 171.1(2) ? . . . . O(1) Mo(1) S(3) C(7) 83.4(4) ? . . . . Mo(2) Mo(1) S(4) C(8) 97.9(4) ? . . . . S(1) Mo(1) S(4) Mo(2) 72.8(2) ? . . . . S(1) Mo(1) S(4) C(8) 170.7(4) ? . . . . S(2) Mo(1) S(4) Mo(2) 1.4(3) ? . . . . S(2) Mo(1) S(4) C(8) 99.3(4) ? . . . . S(3) Mo(1) S(4) Mo(2) -73.4(2) ? . . . . S(3) Mo(1) S(4) C(8) 24.4(4) ? . . . . O(1) Mo(1) S(4) Mo(2) 179.2(2) ? . . . . O(1) Mo(1) S(4) C(8) -83.0(4) ? . . . . Mo(1) Mo(2) S(1) C(1) 92.8(4) ? . . . . S(2) Mo(2) S(1) Mo(1) -65.8(1) ? . . . . S(2) Mo(2) S(1) C(1) 27.0(4) ? . . . . S(3) Mo(2) S(1) Mo(1) -2.2(2) ? . . . . S(3) Mo(2) S(1) C(1) 90.6(5) ? . . . . S(4) Mo(2) S(1) Mo(1) 78.7(2) ? . . . . S(4) Mo(2) S(1) C(1) 171.5(4) ? . . . . O(2) Mo(2) S(1) Mo(1) -170.6(3) ? . . . . O(2) Mo(2) S(1) C(1) -77.8(4) ? . . . . Mo(1) Mo(2) S(2) C(2) -98.2(4) ? . . . . S(1) Mo(2) S(2) Mo(1) 73.7(2) ? . . . . S(1) Mo(2) S(2) C(2) -24.5(4) ? . . . . S(3) Mo(2) S(2) Mo(1) -71.8(2) ? . . . . S(3) Mo(2) S(2) C(2) -170.1(4) ? . . . . S(4) Mo(2) S(2) Mo(1) 1.4(3) ? . . . . S(4) Mo(2) S(2) C(2) -96.8(5) ? . . . . O(2) Mo(2) S(2) Mo(1) 179.8(3) ? . . . . O(2) Mo(2) S(2) C(2) 81.6(4) ? . . . . Mo(1) Mo(2) S(3) C(7) 101.4(4) ? . . . . S(1) Mo(2) S(3) Mo(1) 2.2(2) ? . . . . S(1) Mo(2) S(3) C(7) 103.6(5) ? . . . . S(2) Mo(2) S(3) Mo(1) 65.8(1) ? . . . . S(2) Mo(2) S(3) C(7) 167.2(4) ? . . . . S(4) Mo(2) S(3) Mo(1) -78.5(2) ? . . . . S(4) Mo(2) S(3) C(7) 22.9(4) ? . . . . O(2) Mo(2) S(3) Mo(1) 170.4(3) ? . . . . O(2) Mo(2) S(3) C(7) -88.2(4) ? . . . . Mo(1) Mo(2) S(4) C(8) -91.9(4) ? . . . . S(1) Mo(2) S(4) Mo(1) -71.9(2) ? . . . . S(1) Mo(2) S(4) C(8) -163.7(4) ? . . . . S(2) Mo(2) S(4) Mo(1) -1.3(3) ? . . . . S(2) Mo(2) S(4) C(8) -93.2(5) ? . . . . S(3) Mo(2) S(4) Mo(1) 70.1(2) ? . . . . S(3) Mo(2) S(4) C(8) -21.8(4) ? . . . . O(2) Mo(2) S(4) Mo(1) -179.7(3) ? . . . . O(2) Mo(2) S(4) C(8) 88.5(4) ? . . . . Mo(1) S(1) C(1) C(2) 10(1) ? . . . . Mo(1) S(1) C(1) C(6) -162.7(8) ? . . . . Mo(2) S(1) C(1) C(2) -27(1) ? . . . . Mo(2) S(1) C(1) C(6) 158.7(8) ? . . . . Mo(1) S(2) C(2) C(1) -20(1) ? . . . . Mo(1) S(2) C(2) C(3) 164.2(8) ? . . . . Mo(2) S(2) C(2) C(1) 17(1) ? . . . . Mo(2) S(2) C(2) C(3) -158.0(8) ? . . . . Mo(1) S(3) C(7) C(8) 18(1) ? . . . . Mo(1) S(3) C(7) C(12) -153.6(9) ? . . . . Mo(2) S(3) C(7) C(8) -20(1) ? . . . . Mo(2) S(3) C(7) C(12) 167.6(9) ? . . . . Mo(1) S(4) C(8) C(7) -22.5(9) ? . . . . Mo(1) S(4) C(8) C(9) 159.7(9) ? . . . . Mo(2) S(4) C(8) C(7) 16.9(9) ? . . . . Mo(2) S(4) C(8) C(9) -160.9(9) ? . . . . C(15) N(1) C(13) C(14) 175(1) ? . . . . C(17) N(1) C(13) C(14) 54(1) ? . . . . C(19) N(1) C(13) C(14) -60(1) ? . . . . C(13) N(1) C(15) C(16) 176(1) ? . . . . C(17) N(1) C(15) C(16) -66(1) ? . . . . C(19) N(1) C(15) C(16) 55(1) ? . . . . C(13) N(1) C(17) C(18) 58(1) ? . . . . C(15) N(1) C(17) C(18) -58(1) ? . . . . C(19) N(1) C(17) C(18) 174(1) ? . . . . C(13) N(1) C(19) C(20) -64(1) ? . . . . C(15) N(1) C(19) C(20) 54(1) ? . . . . C(17) N(1) C(19) C(20) -179(1) ? . . . . S(1) C(1) C(2) S(2) 6(1) ? . . . . S(1) C(1) C(2) C(3) -178.4(9) ? . . . . C(6) C(1) C(2) S(2) 179.6(8) ? . . . . C(6) C(1) C(2) C(3) -4(1) ? . . . . S(1) C(1) C(6) Cl(1) -5(1) ? . . . . S(1) C(1) C(6) C(5) 175(1) ? . . . . C(2) C(1) C(6) Cl(1) -179.2(9) ? . . . . C(2) C(1) C(6) C(5) 2(1) ? . . . . S(2) C(2) C(3) Cl(2) -2(1) ? . . . . S(2) C(2) C(3) C(4) -177(1) ? . . . . C(1) C(2) C(3) Cl(2) -178.1(8) ? . . . . C(1) C(2) C(3) C(4) 7(1) ? . . . . Cl(2) C(3) C(4) C(5) 177(1) ? . . . . C(2) C(3) C(4) C(5) -7(1) ? . . . . C(3) C(4) C(5) C(6) 4(1) ? . . . . C(4) C(5) C(6) Cl(1) 179(1) ? . . . . C(4) C(5) C(6) C(1) -2(1) ? . . . . S(3) C(7) C(8) S(4) 3(1) ? . . . . S(3) C(7) C(8) C(9) -178(1) ? . . . . C(12) C(7) C(8) S(4) 176.2(8) ? . . . . C(12) C(7) C(8) C(9) -5(1) ? . . . . S(3) C(7) C(12) Cl(3) -2(1) ? . . . . S(3) C(7) C(12) C(11) 176(1) ? . . . . C(8) C(7) C(12) Cl(3) -175.1(8) ? . . . . C(8) C(7) C(12) C(11) 4(1) ? . . . . S(4) C(8) C(9) Cl(4) 0(1) ? . . . . S(4) C(8) C(9) C(10) -174(1) ? . . . . C(7) C(8) C(9) Cl(4) -178.7(8) ? . . . . C(7) C(8) C(9) C(10) 7(1) ? . . . . Cl(4) C(9) C(10) C(11) 178(1) ? . . . . C(8) C(9) C(10) C(11) -7(1) ? . . . . C(10) C(11) C(12) Cl(3) 175.3(9) ? . . . . #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #============================================================================== data_(Et4N)2[4] _database_code_depnum_ccdc_archive 'CCDC 253879' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C28 H44 Cl4 N2 Mo2 O5 S4 ' _chemical_formula_moiety 'C28 H44 Cl4 N2 Mo2 O5 S4 ' _chemical_formula_weight 950.60 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 1/2-X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 13.6909(8) _cell_length_b 9.9329(5) _cell_length_c 13.9284(8) _cell_angle_alpha 90 _cell_angle_beta 95.652(3) _cell_angle_gamma 90 _cell_volume 1884.9(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 5674 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 123.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 964.00 _exptl_absorpt_coefficient_mu 1.207 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.755 _exptl_absorpt_correction_T_max 0.886 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 30314 _diffrn_reflns_av_R_equivalents 0.027 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9884 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9884 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 4272 _reflns_number_gt 3707 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0720 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 4272 _refine_ls_number_parameters 227 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0004Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 1.84 _refine_diff_density_min -2.13 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mo Mo -1.683 0.686 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo(1) Mo 0.042100(10) 0.04923(2) 0.12809(2) 0.01237(5) Uani 1.00 1 d . . . Cl(1) Cl -0.07842(5) 0.14649(8) 0.48979(5) 0.0251(2) Uani 1.00 1 d . . . Cl(2) Cl -0.28435(5) 0.38287(7) 0.10797(5) 0.0261(2) Uani 1.00 1 d . . . S(1) S -0.00574(4) 0.05699(7) 0.29155(4) 0.0152(1) Uani 1.00 1 d . . . S(2) S -0.11780(4) 0.16523(7) 0.09732(4) 0.0156(2) Uani 1.00 1 d . . . O(1) O 0.12922(13) 0.1711(2) 0.12417(13) 0.0203(5) Uani 1.00 1 d . . . O(2) O 0.1002(1) -0.0960(2) 0.1711(2) 0.0260(5) Uani 1.00 1 d . . . O(3) O 0.0000 0.0000 0.0000 0.0303(8) Uani 1.00 2 d S . . N(1) N 0.9167(2) 0.4693(2) 0.7528(2) 0.0157(5) Uani 1.00 1 d . . . C(1) C -0.1034(2) 0.1707(3) 0.2949(2) 0.0146(6) Uani 1.00 1 d . . . C(2) C -0.1520(2) 0.2204(3) 0.2084(2) 0.0147(6) Uani 1.00 1 d . . . C(3) C -0.2284(2) 0.3126(3) 0.2139(2) 0.0184(6) Uani 1.00 1 d . . . C(4) C -0.2601(2) 0.3511(3) 0.3013(2) 0.0225(7) Uani 1.00 1 d . . . C(5) C -0.2143(2) 0.2989(3) 0.3864(2) 0.0223(7) Uani 1.00 1 d . . . C(6) C -0.1362(2) 0.2107(3) 0.3821(2) 0.0180(6) Uani 1.00 1 d . . . C(7) C 0.8224(2) 0.4118(3) 0.7853(2) 0.0178(6) Uani 1.00 1 d . . . C(8) C 0.7738(2) 0.4975(3) 0.8572(2) 0.0287(8) Uani 1.00 1 d . . . C(9) C 0.8978(2) 0.6022(3) 0.6990(2) 0.0243(7) Uani 1.00 1 d . . . C(10) C 0.8325(2) 0.5928(3) 0.6046(2) 0.0289(8) Uani 1.00 1 d . . . C(11) C 0.9562(2) 0.3639(3) 0.6878(2) 0.0202(7) Uani 1.00 1 d . . . C(12) C 1.0511(2) 0.4022(3) 0.6478(2) 0.0308(8) Uani 1.00 1 d . . . C(13) C 0.9910(2) 0.5002(3) 0.8378(2) 0.0226(7) Uani 1.00 1 d . . . C(14) C 1.0217(2) 0.3808(3) 0.9017(2) 0.0318(8) Uani 1.00 1 d . . . H(1) H -0.3131 0.4126 0.3022 0.028 Uiso 1.00 1 c R . . H(2) H -0.2357 0.3232 0.4468 0.027 Uiso 1.00 1 c R . . H(3) H 0.7769 0.3999 0.7299 0.021 Uiso 1.00 1 c R . . H(4) H 0.8371 0.3269 0.8147 0.021 Uiso 1.00 1 c R . . H(5) H 0.8174 0.5081 0.9141 0.035 Uiso 1.00 1 c R . . H(6) H 0.7590 0.5833 0.8293 0.035 Uiso 1.00 1 c R . . H(7) H 0.7149 0.4559 0.8730 0.035 Uiso 1.00 1 c R . . H(8) H 0.8675 0.6620 0.7403 0.030 Uiso 1.00 1 c R . . H(9) H 0.9593 0.6382 0.6855 0.030 Uiso 1.00 1 c R . . H(10) H 0.8234 0.6798 0.5768 0.035 Uiso 1.00 1 c R . . H(11) H 0.8626 0.5357 0.5614 0.035 Uiso 1.00 1 c R . . H(12) H 0.7706 0.5564 0.6165 0.035 Uiso 1.00 1 c R . . H(13) H 0.9675 0.2838 0.7245 0.024 Uiso 1.00 1 c R . . H(14) H 0.9078 0.3474 0.6354 0.024 Uiso 1.00 1 c R . . H(15) H 1.1005 0.4190 0.6992 0.038 Uiso 1.00 1 c R . . H(16) H 1.0713 0.3306 0.6091 0.038 Uiso 1.00 1 c R . . H(17) H 1.0407 0.4810 0.6096 0.038 Uiso 1.00 1 c R . . H(18) H 1.0481 0.5361 0.8137 0.027 Uiso 1.00 1 c R . . H(19) H 0.9633 0.5659 0.8766 0.027 Uiso 1.00 1 c R . . H(20) H 0.9657 0.3454 0.9280 0.038 Uiso 1.00 1 c R . . H(21) H 1.0491 0.3138 0.8637 0.038 Uiso 1.00 1 c R . . H(22) H 1.0690 0.4076 0.9526 0.038 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mo(1) 0.01210(10) 0.01143(11) 0.01383(11) 0.00094(8) 0.00253(7) -0.00265(8) Cl(1) 0.0299(4) 0.0312(4) 0.0142(3) -0.0012(3) 0.0011(3) -0.0057(3) Cl(2) 0.0249(3) 0.0242(4) 0.0298(4) 0.0115(3) 0.0057(3) 0.0059(3) S(1) 0.0154(3) 0.0163(3) 0.0142(3) 0.0019(2) 0.0022(2) 0.0005(2) S(2) 0.0154(3) 0.0177(3) 0.0140(3) 0.0033(2) 0.0023(2) -0.0006(2) O(1) 0.0170(9) 0.0198(10) 0.0248(10) -0.0027(7) 0.0051(7) -0.0013(8) O(2) 0.0284(10) 0.0196(10) 0.0312(11) 0.0098(8) 0.0099(9) 0.0018(9) O(3) 0.026(2) 0.043(2) 0.021(1) 0.011(1) 0.0005(12) -0.016(1) N(1) 0.0181(10) 0.0131(11) 0.0160(10) -0.0043(8) 0.0016(8) -0.0035(8) C(1) 0.0136(11) 0.0109(12) 0.0198(12) -0.0029(9) 0.0035(9) -0.0027(10) C(2) 0.0146(11) 0.0124(12) 0.0177(12) -0.0025(10) 0.0050(9) -0.0021(10) C(3) 0.0164(12) 0.0136(13) 0.0254(13) 0.0008(10) 0.0028(10) 0.0016(11) C(4) 0.0185(12) 0.020(1) 0.031(2) 0.0040(11) 0.0100(11) -0.0030(12) C(5) 0.0243(13) 0.021(1) 0.024(1) -0.0036(11) 0.0122(11) -0.0090(11) C(6) 0.0201(12) 0.0168(13) 0.0171(12) -0.0047(10) 0.0024(10) -0.0039(10) C(7) 0.0156(12) 0.018(1) 0.0194(12) -0.0047(10) 0.0019(10) 0.0000(10) C(8) 0.025(1) 0.037(2) 0.025(2) -0.0053(13) 0.0084(12) -0.007(1) C(9) 0.033(2) 0.014(1) 0.028(1) -0.0015(12) 0.0111(12) 0.0012(12) C(10) 0.029(2) 0.030(2) 0.028(2) 0.0046(13) 0.0064(12) 0.0109(13) C(11) 0.0238(13) 0.0154(13) 0.0213(13) 0.0008(11) 0.0015(11) -0.0066(11) C(12) 0.029(2) 0.032(2) 0.033(2) 0.0003(13) 0.0119(13) -0.008(1) C(13) 0.0189(13) 0.029(2) 0.0196(13) -0.0096(11) 0.0008(11) -0.0076(12) C(14) 0.027(2) 0.044(2) 0.023(2) -0.003(1) -0.0047(12) -0.001(1) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'DIRDIF99 (PATTY)' _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mo(1) S(1) 2.4315(6) ? . . Mo(1) S(2) 2.4737(6) ? . . Mo(1) O(1) 1.704(2) ? . . Mo(1) O(2) 1.726(2) ? . . Mo(1) O(3) 1.8846(3) ? . . Cl(1) C(6) 1.746(3) ? . . Cl(2) C(3) 1.740(3) ? . . S(1) C(1) 1.754(2) ? . . S(2) C(2) 1.747(3) ? . . O(3) Mo(1) 1.8846(3) ? . 55503 N(1) C(7) 1.521(3) ? . . N(1) C(9) 1.528(3) ? . . N(1) C(11) 1.518(3) ? . . N(1) C(13) 1.514(3) ? . . C(1) C(2) 1.408(3) ? . . C(1) C(6) 1.395(4) ? . . C(2) C(3) 1.399(4) ? . . C(3) C(4) 1.385(4) ? . . C(4) C(5) 1.386(4) ? . . C(5) C(6) 1.387(4) ? . . C(7) C(8) 1.517(4) ? . . C(9) C(10) 1.518(4) ? . . C(11) C(12) 1.512(4) ? . . C(13) C(14) 1.517(4) ? . . C(4) H(1) 0.9500 ? . . C(5) H(2) 0.9501 ? . . C(7) H(3) 0.9499 ? . . C(7) H(4) 0.9500 ? . . C(8) H(5) 0.9500 ? . . C(8) H(6) 0.9500 ? . . C(8) H(7) 0.9500 ? . . C(9) H(8) 0.9499 ? . . C(9) H(9) 0.9500 ? . . C(10) H(10) 0.9500 ? . . C(10) H(11) 0.9500 ? . . C(10) H(12) 0.9500 ? . . C(11) H(13) 0.9500 ? . . C(11) H(14) 0.9500 ? . . C(12) H(15) 0.9500 ? . . C(12) H(16) 0.9500 ? . . C(12) H(17) 0.9499 ? . . C(13) H(18) 0.9501 ? . . C(13) H(19) 0.9500 ? . . C(14) H(20) 0.9500 ? . . C(14) H(21) 0.9500 ? . . C(14) H(22) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 S(2) Mo(1) S(1) 80.33(2) ? . . . O(1) Mo(1) S(1) 105.16(6) ? . . . O(2) Mo(1) S(1) 81.91(7) ? . . . O(3) Mo(1) S(1) 144.01(2) ? . . . Mo(1) S(1) C(1) 108.76(9) ? . . . O(1) Mo(1) S(2) 105.90(7) ? . . . O(2) Mo(1) S(2) 145.02(7) ? . . . O(3) Mo(1) S(2) 76.93(1) ? . . . Mo(1) S(2) C(2) 107.59(8) ? . . . O(2) Mo(1) O(1) 107.72(9) ? . . . O(3) Mo(1) O(1) 107.68(6) ? . . . O(3) Mo(1) O(2) 101.48(7) ? . . . Mo(1) O(3) Mo(1) 180.00(1) ? . . 55503 Cl(1) C(6) C(1) 119.1(2) ? . . . Cl(1) C(6) C(5) 118.7(2) ? . . . Cl(2) C(3) C(2) 119.0(2) ? . . . Cl(2) C(3) C(4) 119.0(2) ? . . . S(1) C(1) C(2) 120.0(2) ? . . . S(1) C(1) C(6) 121.3(2) ? . . . S(2) C(2) C(1) 120.2(2) ? . . . S(2) C(2) C(3) 121.4(2) ? . . . O(3) Mo(1) S(2) 76.93(1) ? . 55503 55503 O(3) Mo(1) O(1) 107.68(6) ? . 55503 55503 O(3) Mo(1) O(2) 101.48(7) ? . 55503 55503 N(1) C(7) C(8) 115.2(2) ? . . . C(9) N(1) C(7) 111.3(2) ? . . . C(11) N(1) C(7) 106.3(2) ? . . . C(13) N(1) C(7) 111.6(2) ? . . . N(1) C(9) C(10) 115.4(2) ? . . . C(11) N(1) C(9) 110.9(2) ? . . . C(13) N(1) C(9) 106.0(2) ? . . . N(1) C(11) C(12) 114.6(2) ? . . . C(13) N(1) C(11) 110.8(2) ? . . . N(1) C(13) C(14) 115.2(2) ? . . . C(6) C(1) C(2) 118.7(2) ? . . . C(1) C(2) C(3) 118.4(2) ? . . . C(1) C(6) C(5) 122.2(2) ? . . . C(2) C(3) C(4) 122.0(2) ? . . . C(3) C(4) C(5) 119.6(2) ? . . . C(4) C(5) C(6) 119.0(3) ? . . . N(1) C(7) H(3) 108.1969 ? . . . N(1) C(7) H(4) 108.1129 ? . . . N(1) C(9) H(8) 107.7438 ? . . . N(1) C(9) H(9) 108.1273 ? . . . N(1) C(11) H(13) 107.8201 ? . . . N(1) C(11) H(14) 108.3339 ? . . . N(1) C(13) H(18) 108.2385 ? . . . N(1) C(13) H(19) 107.9956 ? . . . C(3) C(4) H(1) 119.7116 ? . . . C(4) C(5) H(2) 120.6328 ? . . . H(1) C(4) C(5) 120.6974 ? . . . H(2) C(5) C(6) 120.3405 ? . . . H(3) C(7) C(8) 108.1401 ? . . . H(4) C(7) C(8) 107.6176 ? . . . C(7) C(8) H(5) 109.3711 ? . . . C(7) C(8) H(6) 108.8193 ? . . . C(7) C(8) H(7) 110.2198 ? . . . H(4) C(7) H(3) 109.4614 ? . . . H(6) C(8) H(5) 109.4743 ? . . . H(7) C(8) H(5) 109.4650 ? . . . H(7) C(8) H(6) 109.4747 ? . . . H(8) C(9) C(10) 107.9839 ? . . . H(9) C(9) C(10) 108.0827 ? . . . C(9) C(10) H(10) 109.8087 ? . . . C(9) C(10) H(11) 109.2555 ? . . . C(9) C(10) H(12) 109.3449 ? . . . H(9) C(9) H(8) 109.4575 ? . . . H(11) C(10) H(10) 109.4774 ? . . . H(12) C(10) H(10) 109.4705 ? . . . H(12) C(10) H(11) 109.4697 ? . . . H(13) C(11) C(12) 107.9179 ? . . . H(14) C(11) C(12) 108.6537 ? . . . C(11) C(12) H(15) 109.9060 ? . . . C(11) C(12) H(16) 109.3502 ? . . . C(11) C(12) H(17) 109.1576 ? . . . H(14) C(11) H(13) 109.4613 ? . . . H(16) C(12) H(15) 109.4690 ? . . . H(17) C(12) H(15) 109.4704 ? . . . H(17) C(12) H(16) 109.4733 ? . . . H(18) C(13) C(14) 108.0473 ? . . . H(19) C(13) C(14) 107.8173 ? . . . C(13) C(14) H(20) 109.1550 ? . . . C(13) C(14) H(21) 108.8866 ? . . . C(13) C(14) H(22) 110.3613 ? . . . H(19) C(13) H(18) 109.4622 ? . . . H(21) C(14) H(20) 109.4767 ? . . . H(22) C(14) H(20) 109.4669 ? . . . H(22) C(14) H(21) 109.4771 ? . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 S(2) Mo(1) S(1) C(1) -14.18(9) ? . . . . O(1) Mo(1) S(1) C(1) 89.82(9) ? . . . . O(2) Mo(1) S(1) C(1) -163.92(9) ? . . . . O(3) Mo(1) S(1) C(1) -65.5(1) ? . . . . S(1) Mo(1) S(2) C(2) 14.88(9) ? . . . . O(1) Mo(1) S(2) C(2) -88.26(9) ? . . . . O(2) Mo(1) S(2) C(2) 75.4(1) ? . . . . O(3) Mo(1) S(2) C(2) 166.79(9) ? . . . . Mo(1) S(1) C(1) C(2) 11.5(2) ? . . . . Mo(1) S(1) C(1) C(6) -170.3(2) ? . . . . Mo(1) S(2) C(2) C(1) -14.1(2) ? . . . . Mo(1) S(2) C(2) C(3) 166.9(2) ? . . . . C(9) N(1) C(7) C(8) -63.2(3) ? . . . . C(11) N(1) C(7) C(8) 175.9(2) ? . . . . C(13) N(1) C(7) C(8) 55.0(3) ? . . . . C(7) N(1) C(9) C(10) -64.3(3) ? . . . . C(11) N(1) C(9) C(10) 53.9(3) ? . . . . C(13) N(1) C(9) C(10) 174.2(2) ? . . . . C(7) N(1) C(11) C(12) -179.8(2) ? . . . . C(9) N(1) C(11) C(12) 59.1(3) ? . . . . C(13) N(1) C(11) C(12) -58.4(3) ? . . . . C(7) N(1) C(13) C(14) 59.2(3) ? . . . . C(9) N(1) C(13) C(14) -179.4(2) ? . . . . C(11) N(1) C(13) C(14) -59.1(3) ? . . . . S(1) C(1) C(2) S(2) 1.9(3) ? . . . . S(1) C(1) C(2) C(3) -179.0(2) ? . . . . C(6) C(1) C(2) S(2) -176.3(2) ? . . . . C(6) C(1) C(2) C(3) 2.8(4) ? . . . . S(1) C(1) C(6) Cl(1) 0.2(3) ? . . . . S(1) C(1) C(6) C(5) -179.0(2) ? . . . . C(2) C(1) C(6) Cl(1) 178.4(2) ? . . . . C(2) C(1) C(6) C(5) -0.8(4) ? . . . . S(2) C(2) C(3) Cl(2) -4.8(3) ? . . . . S(2) C(2) C(3) C(4) 176.1(2) ? . . . . C(1) C(2) C(3) Cl(2) 176.1(2) ? . . . . C(1) C(2) C(3) C(4) -3.0(4) ? . . . . Cl(2) C(3) C(4) C(5) -178.1(2) ? . . . . C(2) C(3) C(4) C(5) 1.0(4) ? . . . . C(3) C(4) C(5) C(6) 1.2(4) ? . . . . C(4) C(5) C(6) Cl(1) 179.5(2) ? . . . . C(4) C(5) C(6) C(1) -1.2(4) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 Mo(1) C(1) 3.425(3) ? . . Mo(1) C(2) 3.433(2) ? . . Cl(1) Cl(2) 3.426(1) ? . 44502 Cl(1) S(1) 3.1537(9) ? . . Cl(1) C(1) 2.713(3) ? . . Cl(1) C(5) 2.702(3) ? . . Cl(1) C(11) 3.498(3) ? . 45501 Cl(2) Cl(1) 3.426(1) ? . 45502 Cl(2) S(2) 3.1562(9) ? . . Cl(2) C(1) 3.574(3) ? . 45502 Cl(2) C(2) 2.710(2) ? . . Cl(2) C(4) 2.698(3) ? . . Cl(2) C(6) 3.440(3) ? . 45502 S(1) S(2) 3.1640(8) ? . . S(1) O(1) 3.314(2) ? . . S(1) O(2) 2.776(2) ? . . S(1) C(2) 2.744(2) ? . . S(1) C(6) 2.750(3) ? . . S(2) O(1) 3.366(2) ? . . S(2) O(3) 2.7500(6) ? . . S(2) C(1) 2.740(3) ? . . S(2) C(3) 2.749(3) ? . . O(1) O(2) 2.770(3) ? . . O(1) O(3) 2.899(2) ? . . O(1) C(7) 3.397(3) ? . 45404 O(1) C(8) 3.550(4) ? . 66603 O(1) C(9) 3.384(3) ? . 66603 O(2) O(3) 2.797(2) ? . . O(2) C(7) 3.348(3) ? . 65603 O(2) C(8) 3.480(3) ? . 45404 O(2) C(10) 3.398(4) ? . 45404 O(2) C(11) 3.441(3) ? . 65603 O(2) C(14) 3.389(4) ? . 65603 O(3) S(2) 2.7500(6) ? . 55503 O(3) O(1) 2.899(2) ? . 55503 O(3) O(2) 2.797(2) ? . 55503 N(1) C(8) 2.565(4) ? . . N(1) C(10) 2.574(4) ? . . N(1) C(12) 2.549(4) ? . . N(1) C(14) 2.560(4) ? . . C(1) Cl(2) 3.574(3) ? . 44502 C(1) C(3) 2.411(3) ? . . C(1) C(4) 2.804(4) ? . . C(1) C(5) 2.436(4) ? . . C(2) C(4) 2.435(4) ? . . C(2) C(5) 2.811(4) ? . . C(2) C(6) 2.410(4) ? . . C(3) C(5) 2.395(4) ? . . C(3) C(6) 2.743(4) ? . . C(4) C(6) 2.390(4) ? . . C(6) Cl(2) 3.440(3) ? . 44502 C(7) O(1) 3.397(3) ? . 55504 C(7) O(2) 3.348(3) ? . 65603 C(7) C(9) 2.517(4) ? . . C(7) C(10) 3.107(4) ? . . C(7) C(11) 2.433(4) ? . . C(7) C(13) 2.511(4) ? . . C(7) C(14) 3.049(4) ? . . C(8) O(1) 3.550(4) ? . 66603 C(8) O(2) 3.480(3) ? . 55504 C(8) C(9) 3.092(4) ? . . C(8) C(13) 3.013(4) ? . . C(8) C(14) 3.583(4) ? . . C(9) O(1) 3.384(3) ? . 66603 C(9) C(11) 2.509(4) ? . . C(9) C(12) 3.026(4) ? . . C(9) C(13) 2.430(4) ? . . C(10) O(2) 3.398(4) ? . 55504 C(10) C(11) 2.999(4) ? . . C(10) C(12) 3.542(4) ? . . C(11) Cl(1) 3.498(3) ? . 65501 C(11) O(2) 3.441(3) ? . 65603 C(11) C(13) 2.496(4) ? . . C(11) C(14) 3.030(4) ? . . C(12) C(13) 3.009(4) ? . . C(14) O(2) 3.389(4) ? . 65603 Mo(1) H(3) 3.4210 ? . 45404 Mo(1) H(8) 3.5597 ? . 66603 Mo(1) H(12) 3.3193 ? . 45404 Cl(1) H(2) 2.7976 ? . . Cl(1) H(7) 3.3810 ? . 54602 Cl(1) H(13) 3.5409 ? . 45501 Cl(1) H(14) 2.8651 ? . 45501 Cl(1) H(16) 3.1046 ? . 45501 Cl(2) H(1) 2.7881 ? . . Cl(2) H(5) 3.3944 ? . 45401 Cl(2) H(7) 3.3511 ? . 45401 Cl(2) H(10) 3.2726 ? . 54502 Cl(2) H(16) 2.8995 ? . 35404 Cl(2) H(18) 3.4065 ? . 66603 S(1) H(1) 3.0454 ? . 44502 S(1) H(7) 3.1238 ? . 45404 S(1) H(8) 3.4259 ? . 66603 S(1) H(9) 3.1039 ? . 66603 S(1) H(13) 3.4358 ? . 65603 S(2) H(1) 3.0672 ? . 44502 S(2) H(10) 3.5330 ? . 54502 S(2) H(18) 3.3190 ? . 66603 S(2) H(19) 3.4044 ? . 66603 S(2) H(20) 3.2559 ? . 45401 O(1) H(2) 3.2282 ? . 55404 O(1) H(3) 2.4836 ? . 45404 O(1) H(5) 3.3240 ? . 66603 O(1) H(6) 2.9191 ? . 66603 O(1) H(8) 2.5094 ? . 66603 O(1) H(9) 3.5660 ? . 66603 O(1) H(12) 2.9845 ? . 45404 O(1) H(19) 2.9030 ? . 66603 O(1) H(22) 3.3945 ? . 45401 O(2) H(3) 3.1505 ? . 45404 O(2) H(4) 2.4504 ? . 65603 O(2) H(6) 2.9417 ? . 45404 O(2) H(7) 3.3829 ? . 45404 O(2) H(10) 3.5410 ? . 45404 O(2) H(12) 2.5543 ? . 45404 O(2) H(13) 2.5927 ? . 65603 O(2) H(20) 2.9339 ? . 65603 O(2) H(21) 2.9832 ? . 65603 O(3) H(20) 3.5920 ? . 45401 O(3) H(20) 3.5920 ? . 65603 N(1) H(3) 2.0294 ? . . N(1) H(4) 2.0285 ? . . N(1) H(5) 2.7644 ? . . N(1) H(6) 2.7441 ? . . N(1) H(7) 3.3702 ? . . N(1) H(8) 2.0301 ? . . N(1) H(9) 2.0346 ? . . N(1) H(10) 3.3754 ? . . N(1) H(11) 2.7747 ? . . N(1) H(12) 2.7570 ? . . N(1) H(13) 2.0225 ? . . N(1) H(14) 2.0286 ? . . N(1) H(15) 2.7405 ? . . N(1) H(16) 3.3505 ? . . N(1) H(17) 2.7474 ? . . N(1) H(18) 2.0239 ? . . N(1) H(19) 2.0210 ? . . N(1) H(20) 2.7560 ? . . N(1) H(21) 2.7404 ? . . N(1) H(22) 3.3651 ? . . C(1) H(1) 3.0664 ? . 44502 C(1) H(2) 3.2888 ? . . C(1) H(9) 2.7317 ? . 66603 C(1) H(18) 3.4013 ? . 66603 C(2) H(1) 3.2852 ? . . C(2) H(1) 3.0953 ? . 44502 C(2) H(9) 3.2167 ? . 66603 C(2) H(18) 2.8378 ? . 66603 C(3) H(1) 2.0315 ? . . C(3) H(2) 3.2579 ? . . C(3) H(15) 3.3505 ? . 66603 C(3) H(15) 3.2750 ? . 35404 C(3) H(16) 3.2988 ? . 35404 C(3) H(18) 2.9475 ? . 66603 C(4) H(2) 2.0410 ? . . C(4) H(15) 3.1612 ? . 66603 C(4) H(15) 3.5112 ? . 35404 C(4) H(17) 3.5508 ? . 66603 C(4) H(21) 3.2726 ? . 35404 C(5) H(1) 2.0416 ? . . C(5) H(11) 3.4753 ? . 45501 C(5) H(15) 3.4736 ? . 66603 C(5) H(17) 3.2251 ? . 66603 C(5) H(21) 3.4123 ? . 35404 C(6) H(1) 3.2548 ? . . C(6) H(2) 2.0394 ? . . C(6) H(9) 3.0754 ? . 66603 C(6) H(17) 3.3271 ? . 66603 C(7) H(5) 2.0395 ? . . C(7) H(6) 2.0331 ? . . C(7) H(7) 2.0493 ? . . C(7) H(8) 2.6504 ? . . C(7) H(8) 3.5865 ? . 64602 C(7) H(9) 3.3190 ? . . C(7) H(11) 3.4468 ? . . C(7) H(12) 2.7865 ? . . C(7) H(13) 2.5724 ? . . C(7) H(14) 2.5724 ? . . C(7) H(18) 3.3153 ? . . C(7) H(19) 2.6828 ? . . C(7) H(20) 2.7321 ? . . C(7) H(21) 3.3333 ? . . C(8) H(3) 2.0251 ? . . C(8) H(4) 2.0189 ? . . C(8) H(8) 2.7161 ? . . C(8) H(10) 3.5795 ? . 64602 C(8) H(12) 3.3992 ? . . C(8) H(19) 2.6695 ? . . C(8) H(20) 3.1061 ? . . C(9) H(3) 2.6656 ? . . C(9) H(4) 3.3211 ? . . C(9) H(5) 3.4222 ? . . C(9) H(6) 2.7607 ? . . C(9) H(10) 2.0456 ? . . C(9) H(11) 2.0392 ? . . C(9) H(12) 2.0402 ? . . C(9) H(13) 3.3131 ? . . C(9) H(14) 2.6898 ? . . C(9) H(15) 3.3184 ? . . C(9) H(17) 2.7041 ? . . C(9) H(18) 2.5635 ? . . C(9) H(19) 2.5728 ? . . C(10) H(2) 3.5309 ? . 65501 C(10) H(3) 2.7492 ? . . C(10) H(4) 3.5463 ? . 65602 C(10) H(6) 3.3816 ? . . C(10) H(8) 2.0242 ? . . C(10) H(9) 2.0254 ? . . C(10) H(14) 2.6651 ? . . C(10) H(16) 3.4557 ? . 76603 C(10) H(17) 3.0541 ? . . C(11) H(3) 2.6037 ? . . C(11) H(4) 2.5459 ? . . C(11) H(8) 3.3089 ? . . C(11) H(9) 2.7251 ? . . C(11) H(11) 2.6846 ? . . C(11) H(12) 3.2555 ? . . C(11) H(15) 2.0410 ? . . C(11) H(16) 2.0346 ? . . C(11) H(17) 2.0323 ? . . C(11) H(18) 2.6737 ? . . C(11) H(19) 3.3018 ? . . C(11) H(20) 3.3398 ? . . C(11) H(21) 2.6935 ? . . C(12) H(9) 2.7351 ? . . C(12) H(11) 3.0417 ? . . C(12) H(11) 3.3093 ? . 76603 C(12) H(13) 2.0178 ? . . C(12) H(14) 2.0265 ? . . C(12) H(18) 2.6698 ? . . C(12) H(21) 3.1353 ? . . C(13) H(3) 3.3127 ? . . C(13) H(4) 2.7155 ? . . C(13) H(5) 2.6981 ? . . C(13) H(6) 3.2726 ? . . C(13) H(8) 2.6129 ? . . C(13) H(9) 2.5261 ? . . C(13) H(13) 2.6676 ? . . C(13) H(14) 3.3036 ? . . C(13) H(15) 2.6823 ? . . C(13) H(17) 3.3216 ? . . C(13) H(20) 2.0374 ? . . C(13) H(21) 2.0343 ? . . C(13) H(22) 2.0514 ? . . C(14) H(4) 2.7459 ? . . C(14) H(5) 3.0898 ? . . C(14) H(13) 2.6846 ? . . C(14) H(15) 3.1397 ? . . C(14) H(18) 2.0245 ? . . C(14) H(19) 2.0217 ? . . H(1) S(1) 3.0454 ? . 45502 H(1) S(2) 3.0672 ? . 45502 H(1) C(1) 3.0664 ? . 45502 H(1) C(2) 3.0953 ? . 45502 H(2) O(1) 3.2282 ? . 45504 H(2) C(10) 3.5309 ? . 45501 H(3) Mo(1) 3.4210 ? . 55504 H(3) O(1) 2.4836 ? . 55504 H(3) O(2) 3.1505 ? . 55504 H(4) O(2) 2.4504 ? . 65603 H(4) C(10) 3.5463 ? . 64602 H(5) Cl(2) 3.3944 ? . 65601 H(5) O(1) 3.3240 ? . 66603 H(6) O(1) 2.9191 ? . 66603 H(6) O(2) 2.9417 ? . 55504 H(7) Cl(1) 3.3810 ? . 55602 H(7) Cl(2) 3.3511 ? . 65601 H(7) S(1) 3.1238 ? . 55504 H(7) O(2) 3.3829 ? . 55504 H(8) Mo(1) 3.5597 ? . 66603 H(8) S(1) 3.4259 ? . 66603 H(8) O(1) 2.5094 ? . 66603 H(8) C(7) 3.5865 ? . 65602 H(9) S(1) 3.1039 ? . 66603 H(9) O(1) 3.5660 ? . 66603 H(9) C(1) 2.7317 ? . 66603 H(9) C(2) 3.2167 ? . 66603 H(9) C(6) 3.0754 ? . 66603 H(10) Cl(2) 3.2726 ? . 55502 H(10) S(2) 3.5330 ? . 55502 H(10) O(2) 3.5410 ? . 55504 H(10) C(8) 3.5795 ? . 65602 H(11) C(5) 3.4753 ? . 65501 H(11) C(12) 3.3093 ? . 76603 H(12) Mo(1) 3.3193 ? . 55504 H(12) O(1) 2.9845 ? . 55504 H(12) O(2) 2.5543 ? . 55504 H(13) Cl(1) 3.5409 ? . 65501 H(13) S(1) 3.4358 ? . 65603 H(13) O(2) 2.5927 ? . 65603 H(14) Cl(1) 2.8651 ? . 65501 H(15) C(3) 3.3505 ? . 66603 H(15) C(3) 3.2750 ? . 65504 H(15) C(4) 3.1612 ? . 66603 H(15) C(4) 3.5112 ? . 65504 H(15) C(5) 3.4736 ? . 66603 H(16) Cl(1) 3.1046 ? . 65501 H(16) Cl(2) 2.8995 ? . 65504 H(16) C(3) 3.2988 ? . 65504 H(16) C(10) 3.4557 ? . 76603 H(17) C(4) 3.5508 ? . 66603 H(17) C(5) 3.2251 ? . 66603 H(17) C(6) 3.3271 ? . 66603 H(18) Cl(2) 3.4065 ? . 66603 H(18) S(2) 3.3190 ? . 66603 H(18) C(1) 3.4013 ? . 66603 H(18) C(2) 2.8378 ? . 66603 H(18) C(3) 2.9475 ? . 66603 H(19) S(2) 3.4044 ? . 66603 H(19) O(1) 2.9030 ? . 66603 H(20) S(2) 3.2559 ? . 65601 H(20) O(2) 2.9339 ? . 65603 H(20) O(3) 3.5920 ? . 65601 H(21) O(2) 2.9832 ? . 65603 H(21) C(4) 3.2726 ? . 65504 H(21) C(5) 3.4123 ? . 65504 H(22) O(1) 3.3945 ? . 65601 #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #============================================================================== data_[5] _database_code_depnum_ccdc_archive 'CCDC 253880' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C12 H4 Cl4 S4 ' _chemical_formula_moiety 'C12 H4 Cl4 S4 ' _chemical_formula_weight 418.22 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,1/2+Y,1/2-Z 3 -X,-Y,-Z 4 +X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 4.289(2) _cell_length_b 13.968(5) _cell_length_c 11.991(5) _cell_angle_alpha 90 _cell_angle_beta 93.528(8) _cell_angle_gamma 90 _cell_volume 717.1(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 2439 _cell_measurement_theta_min 3.4 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 123.1 #------------------------------------------------------------------------------ _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.31 _exptl_crystal_density_diffrn 1.937 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 416.00 _exptl_absorpt_coefficient_mu 1.388 _exptl_absorpt_correction_type psi-scans _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.327 _exptl_absorpt_correction_T_max 0.650 #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 3430 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9936 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9936 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 1638 _reflns_number_gt 1184 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.2510 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 1638 _refine_ls_number_parameters 93 _refine_ls_goodness_of_fit_ref 0.969 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0074Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 2.08 _refine_diff_density_min -1.00 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Cl Cl 0.148 0.159 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS 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 Cl(1) Cl 0.4835(4) 0.32053(12) 0.9873(2) 0.0314(4) Uani 1.00 1 d . . . Cl(2) Cl 0.0073(4) 0.00926(12) 0.64741(13) 0.0305(4) Uani 1.00 1 d . . . S(1) S 0.4809(4) -0.05726(11) 0.84785(13) 0.0249(4) Uani 1.00 1 d . . . S(2) S 0.7559(4) 0.10976(12) 1.02060(13) 0.0241(4) Uani 1.00 1 d . . . C(1) C 0.360(2) 0.0635(4) 0.8362(5) 0.022(1) Uani 1.00 1 d . . . C(2) C 0.4664(13) 0.1342(5) 0.9125(5) 0.020(1) Uani 1.00 1 d . . . C(3) C 0.360(2) 0.2294(4) 0.8956(5) 0.022(1) Uani 1.00 1 d . . . C(4) C 0.149(2) 0.2544(5) 0.8081(6) 0.027(2) Uani 1.00 1 d . . . C(5) C 0.050(2) 0.1857(5) 0.7327(5) 0.026(2) Uani 1.00 1 d . . . C(6) C 0.147(1) 0.0916(4) 0.7478(5) 0.020(1) Uani 1.00 1 d . . . H(1) H 0.0752 0.3183 0.8006 0.033 Uiso 1.00 1 c R . . H(2) H -0.0843 0.2022 0.6697 0.031 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl(1) 0.0407(10) 0.0205(8) 0.0326(9) 0.0032(6) -0.0018(7) -0.0044(6) Cl(2) 0.0458(10) 0.0191(8) 0.0260(8) -0.0031(6) -0.0027(7) 0.0007(6) S(1) 0.0324(9) 0.0189(8) 0.0241(8) 0.0050(6) 0.0077(6) 0.0011(6) S(2) 0.0230(8) 0.0229(8) 0.0265(8) 0.0005(6) 0.0015(6) 0.0045(6) C(1) 0.024(3) 0.017(3) 0.026(3) -0.000(2) 0.010(3) 0.002(2) C(2) 0.019(3) 0.020(3) 0.021(3) 0.001(2) 0.003(2) 0.006(2) C(3) 0.029(3) 0.015(3) 0.021(3) -0.003(2) 0.004(2) -0.007(2) C(4) 0.034(4) 0.018(3) 0.032(3) 0.001(2) 0.011(3) 0.001(3) C(5) 0.030(3) 0.023(3) 0.024(3) 0.002(3) -0.000(3) 0.004(3) C(6) 0.024(3) 0.018(3) 0.019(3) -0.001(2) 0.007(2) 0.002(2) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution ? _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Cl(1) C(3) 1.743(6) ? . . Cl(2) C(6) 1.744(6) ? . . S(1) C(1) 1.768(6) ? . . S(2) C(2) 1.772(6) ? . . C(1) C(2) 1.402(9) ? . . C(1) C(6) 1.412(8) ? . . C(2) C(3) 1.418(9) ? . . C(3) C(4) 1.386(9) ? . . C(4) C(5) 1.368(9) ? . . C(5) C(6) 1.389(9) ? . . C(4) H(1) 0.9500 ? . . C(5) H(2) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 Cl(1) C(3) C(2) 120.8(4) ? . . . Cl(1) C(3) C(4) 116.9(5) ? . . . Cl(2) C(6) C(1) 121.0(5) ? . . . Cl(2) C(6) C(5) 116.5(5) ? . . . S(1) C(1) C(2) 122.6(5) ? . . . S(1) C(1) C(6) 119.8(5) ? . . . S(2) C(2) C(3) 119.4(5) ? . . . S(2) C(2) C(1) 121.8(5) ? . . . C(1) C(2) C(3) 118.6(5) ? . . . C(6) C(1) C(2) 117.7(5) ? . . . C(1) C(6) C(5) 122.4(6) ? . . . C(2) C(3) C(4) 122.3(6) ? . . . C(3) C(4) C(5) 119.0(6) ? . . . C(4) C(5) C(6) 120.0(6) ? . . . C(3) C(4) H(1) 120.4245 ? . . . H(1) C(4) C(5) 120.5273 ? . . . C(4) C(5) H(2) 120.3195 ? . . . H(2) C(5) C(6) 119.7118 ? . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 S(1) C(1) C(2) S(2) 5.4(8) ? . . . . S(1) C(1) C(2) C(3) 179.3(5) ? . . . . C(6) C(1) C(2) S(2) -175.2(5) ? . . . . C(6) C(1) C(2) C(3) -1.3(9) ? . . . . S(1) C(1) C(6) Cl(2) -1.6(8) ? . . . . S(1) C(1) C(6) C(5) -178.4(6) ? . . . . C(2) C(1) C(6) Cl(2) 179.0(5) ? . . . . C(2) C(1) C(6) C(5) 2.1(9) ? . . . . S(2) C(2) C(3) Cl(1) -5.8(8) ? . . . . S(2) C(2) C(3) C(4) 175.6(6) ? . . . . C(1) C(2) C(3) Cl(1) -179.8(4) ? . . . . C(1) C(2) C(3) C(4) 1(1) ? . . . . Cl(1) C(3) C(4) C(5) 178.8(6) ? . . . . C(2) C(3) C(4) C(5) -2(1) ? . . . . C(3) C(4) C(5) C(6) 3(1) ? . . . . C(4) C(5) C(6) Cl(2) 179.8(4) ? . . . . C(4) C(5) C(6) C(1) -3(1) ? . . . . #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF #============================================================================== #============================================================================== data_(Et3NH)2[6] _database_code_depnum_ccdc_archive 'CCDC 253881' #============================================================================== # CHEMICAL DATA _chemical_formula_sum 'C24 H40 N2 Mo O4 S2 ' _chemical_formula_moiety 'C24 H40 N2 Mo O4 S2 ' _chemical_formula_weight 580.65 _chemical_melting_point ? #============================================================================== # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_site_id _symmetry_equiv_pos_as_xyz 1 +X,+Y,+Z 2 -X,+Y,1/2-Z 3 -X,-Y,-Z 4 +X,-Y,1/2+Z 5 1/2+X,1/2+Y,+Z 6 1/2-X,1/2+Y,1/2-Z 7 1/2-X,1/2-Y,-Z 8 1/2+X,1/2-Y,1/2+Z #------------------------------------------------------------------------------ _cell_length_a 20.287(2) _cell_length_b 10.5551(6) _cell_length_c 12.7613(10) _cell_angle_alpha 90 _cell_angle_beta 99.694(4) _cell_angle_gamma 90 _cell_volume 2693.5(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 4489 _cell_measurement_theta_min 4.0 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 123.1 #------------------------------------------------------------------------------ _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1216.00 _exptl_absorpt_coefficient_mu 0.672 _exptl_absorpt_correction_type none #============================================================================== # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku Mercury' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 6436 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9856 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9856 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 #============================================================================== # REFINEMENT DATA _refine_special_details ; Refinement using all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 3051 _reflns_number_gt 2814 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0710 _refine_ls_hydrogen_treatment refall _refine_ls_number_reflns 3051 _refine_ls_number_parameters 170 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[0.0006Fo^2^ + 1.0000\s(Fo^2^)]/(4Fo^2^)' _refine_ls_shift/su_max 0.0000 _refine_diff_density_max 0.60 _refine_diff_density_min -0.32 _refine_ls_extinction_method none _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.003 0.002 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.000 0.000 ; International Tables for Crystallography (1992, Vol. C, Table 6.1.1.4) ; Mo Mo -1.683 0.686 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.006 0.003 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.011 0.006 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; S S 0.125 0.123 ; International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; #============================================================================== # ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo(1) Mo 0.0000 0.23624(2) 0.2500 0.01161(5) Uani 1.00 2 d S . . S(1) S 0.09922(2) 0.26076(4) 0.16166(3) 0.01779(11) Uani 1.00 1 d . . . O(1) O 0.02282(5) 0.13146(11) 0.35507(9) 0.0163(3) Uani 1.00 1 d . . . O(2) O 0.05418(6) 0.37900(11) 0.33643(9) 0.0165(3) Uani 1.00 1 d . . . N(1) N 0.09792(7) 0.2045(1) 0.54754(11) 0.0166(3) Uani 1.00 1 d . . . C(1) C 0.14185(8) 0.3844(2) 0.2355(1) 0.0175(4) Uani 1.00 1 d . . . C(2) C 0.11042(8) 0.4337(2) 0.31753(13) 0.0161(4) Uani 1.00 1 d . . . C(3) C 0.13966(9) 0.5370(2) 0.3774(1) 0.0204(4) Uani 1.00 1 d . . . C(4) C 0.19901(9) 0.5888(2) 0.3562(2) 0.0251(5) Uani 1.00 1 d . . . C(5) C 0.23012(9) 0.5390(2) 0.2762(2) 0.0266(5) Uani 1.00 1 d . . . C(6) C 0.20158(9) 0.4373(2) 0.2160(2) 0.0232(5) Uani 1.00 1 d . . . C(7) C 0.16904(9) 0.1833(2) 0.5347(2) 0.0321(6) Uani 1.00 1 d . . . C(8) C 0.17780(11) 0.0768(3) 0.4625(2) 0.0637(9) Uani 1.00 1 d . . . C(9) C 0.06947(10) 0.1038(2) 0.6098(1) 0.0247(5) Uani 1.00 1 d . . . C(10) C 0.09561(10) 0.1077(2) 0.7286(1) 0.0253(5) Uani 1.00 1 d . . . C(11) C 0.09075(9) 0.3350(2) 0.59019(13) 0.0226(4) Uani 1.00 1 d . . . C(12) C 0.01955(11) 0.3687(2) 0.5966(2) 0.0333(6) Uani 1.00 1 d . . . H(1) H 0.1188 0.5700 0.4328 0.024 Uiso 1.00 1 c R . . H(2) H 0.2185 0.6587 0.3969 0.029 Uiso 1.00 1 c R . . H(3) H 0.2710 0.5740 0.2628 0.032 Uiso 1.00 1 c R . . H(4) H 0.2223 0.4038 0.1605 0.028 Uiso 1.00 1 c R . . H(5) H 0.1847 0.2580 0.5054 0.039 Uiso 1.00 1 c R . . H(6) H 0.1949 0.1677 0.6027 0.038 Uiso 1.00 1 c R . . H(7) H 0.1624 0.0014 0.4910 0.074 Uiso 1.00 1 c R . . H(8) H 0.1526 0.0918 0.3938 0.074 Uiso 1.00 1 c R . . H(9) H 0.2237 0.0679 0.4573 0.074 Uiso 1.00 1 c R . . H(10) H 0.0223 0.1135 0.5993 0.029 Uiso 1.00 1 c R . . H(11) H 0.0802 0.0235 0.5834 0.029 Uiso 1.00 1 c R . . H(12) H 0.0764 0.0414 0.7637 0.030 Uiso 1.00 1 c R . . H(13) H 0.1428 0.0981 0.7400 0.030 Uiso 1.00 1 c R . . H(14) H 0.0845 0.1871 0.7561 0.030 Uiso 1.00 1 c R . . H(15) H 0.1168 0.3404 0.6593 0.026 Uiso 1.00 1 c R . . H(16) H 0.1069 0.3944 0.5446 0.026 Uiso 1.00 1 c R . . H(17) H 0.0177 0.4521 0.6239 0.039 Uiso 1.00 1 c R . . H(18) H -0.0070 0.3642 0.5279 0.039 Uiso 1.00 1 c R . . H(19) H 0.0029 0.3104 0.6426 0.039 Uiso 1.00 1 c R . . H(20) H 0.0722 0.2031 0.4781 0.020 Uiso 1.00 1 c 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Mo(1) 0.01178(11) 0.01146(11) 0.01105(11) 0.0000 0.00040(7) 0.0000 S(1) 0.0166(2) 0.0188(2) 0.0187(2) 0.0011(1) 0.0053(2) -0.0014(2) O(1) 0.0164(6) 0.0164(6) 0.0147(6) -0.0014(4) -0.0012(4) 0.0001(5) O(2) 0.0160(6) 0.0169(6) 0.0172(6) -0.0049(4) 0.0044(4) -0.0034(5) N(1) 0.0157(7) 0.0210(7) 0.0123(7) 0.0018(5) 0.0001(5) -0.0008(6) C(1) 0.0152(8) 0.0162(8) 0.0206(8) 0.0014(6) 0.0012(6) 0.0040(6) C(2) 0.0144(8) 0.0149(8) 0.0181(8) -0.0013(6) -0.0003(6) 0.0044(6) C(3) 0.0222(9) 0.0180(9) 0.0197(8) -0.0030(7) 0.0003(7) 0.0022(7) C(4) 0.0223(9) 0.0200(9) 0.0296(10) -0.0070(7) -0.0057(7) 0.0054(8) C(5) 0.0147(8) 0.0257(10) 0.0384(11) -0.0046(7) 0.0018(7) 0.0103(8) C(6) 0.0151(8) 0.0255(9) 0.0298(10) 0.0023(7) 0.0060(7) 0.0072(8) C(7) 0.0190(9) 0.056(1) 0.0210(9) 0.0073(9) 0.0033(7) -0.0023(9) C(8) 0.0284(12) 0.113(3) 0.044(1) 0.030(1) -0.0103(10) -0.042(2) C(9) 0.0332(10) 0.0152(9) 0.0249(10) -0.0048(7) 0.0026(8) 0.0006(7) C(10) 0.0331(10) 0.0208(9) 0.0217(9) 0.0004(7) 0.0041(8) 0.0064(7) C(11) 0.0341(10) 0.0170(9) 0.0151(8) -0.0060(7) -0.0007(7) 0.0021(7) C(12) 0.0459(12) 0.0292(11) 0.0222(10) 0.0169(9) -0.0011(8) -0.0034(8) #============================================================================== _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution ? _computing_structure_refinement CRYSTALS _computing_publication_material 'CrystalStructure 3.6.0' _computing_molecular_graphics ? #============================================================================== # MOLECULAR GEOMETRY _geom_special_details ; ENTER SPECIAL DETAILS OF THE MOLECULAR GEOMETRY ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 Mo(1) S(1) 2.4806(4) ? . . Mo(1) S(1) 2.4806(4) ? . 55502 Mo(1) O(1) 1.740(1) ? . . Mo(1) O(1) 1.740(1) ? . 55502 Mo(1) O(2) 2.070(1) ? . . Mo(1) O(2) 2.070(1) ? . 55502 S(1) C(1) 1.751(2) ? . . O(2) C(2) 1.336(2) ? . . N(1) C(7) 1.496(2) ? . . N(1) C(9) 1.500(2) ? . . N(1) C(11) 1.497(2) ? . . C(1) C(2) 1.413(3) ? . . C(1) C(6) 1.394(3) ? . . C(2) C(3) 1.404(2) ? . . C(3) C(4) 1.390(3) ? . . C(4) C(5) 1.390(3) ? . . C(5) C(6) 1.389(3) ? . . C(7) C(8) 1.483(4) ? . . C(9) C(10) 1.520(2) ? . . C(11) C(12) 1.503(3) ? . . N(1) H(20) 0.9499 ? . . C(3) H(1) 0.9500 ? . . C(4) H(2) 0.9500 ? . . C(5) H(3) 0.9501 ? . . C(6) H(4) 0.9500 ? . . C(7) H(5) 0.9500 ? . . C(7) H(6) 0.9500 ? . . C(8) H(7) 0.9499 ? . . C(8) H(8) 0.9500 ? . . C(8) H(9) 0.9500 ? . . C(9) H(10) 0.9501 ? . . C(9) H(11) 0.9499 ? . . C(10) H(12) 0.9500 ? . . C(10) H(13) 0.9500 ? . . C(10) H(14) 0.9500 ? . . C(11) H(15) 0.9500 ? . . C(11) H(16) 0.9500 ? . . C(12) H(17) 0.9500 ? . . C(12) H(18) 0.9500 ? . . C(12) H(19) 0.9500 ? . . loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 S(1) Mo(1) S(1) 168.02(2) ? 55502 . . O(1) Mo(1) S(1) 106.60(4) ? . . . O(1) Mo(1) S(1) 81.20(4) ? 55502 . . O(2) Mo(1) S(1) 76.56(4) ? . . . O(2) Mo(1) S(1) 94.62(4) ? 55502 . . Mo(1) S(1) C(1) 101.43(6) ? . . . O(1) Mo(1) S(1) 81.20(4) ? . . 55502 O(1) Mo(1) S(1) 106.60(4) ? 55502 . 55502 O(2) Mo(1) S(1) 94.62(4) ? . . 55502 O(2) Mo(1) S(1) 76.56(4) ? 55502 . 55502 Mo(1) S(1) C(1) 101.43(6) ? . 55502 55502 O(1) Mo(1) O(1) 101.05(5) ? 55502 . . O(2) Mo(1) O(1) 90.21(5) ? . . . O(2) Mo(1) O(1) 157.19(5) ? 55502 . . O(2) Mo(1) O(1) 157.19(5) ? . . 55502 O(2) Mo(1) O(1) 90.21(5) ? 55502 . 55502 O(2) Mo(1) O(2) 86.60(4) ? 55502 . . Mo(1) O(2) C(2) 127.7(1) ? . . . Mo(1) O(2) C(2) 127.7(1) ? . 55502 55502 S(1) C(1) C(2) 115.4(1) ? . . . S(1) C(1) C(6) 124.6(1) ? . . . O(2) C(2) C(1) 118.7(1) ? . . . O(2) C(2) C(3) 122.2(2) ? . . . N(1) C(7) C(8) 113.6(2) ? . . . C(9) N(1) C(7) 114.6(1) ? . . . C(11) N(1) C(7) 109.4(1) ? . . . C(11) N(1) C(9) 113.0(1) ? . . . N(1) C(9) C(10) 114.1(1) ? . . . N(1) C(11) C(12) 113.0(1) ? . . . C(6) C(1) C(2) 120.0(2) ? . . . C(1) C(2) C(3) 119.1(2) ? . . . C(1) C(6) C(5) 120.3(2) ? . . . C(2) C(3) C(4) 120.0(2) ? . . . C(3) C(4) C(5) 120.6(2) ? . . . C(4) C(5) C(6) 120.0(2) ? . . . H(20) N(1) C(7) 106.4191 ? . . . N(1) C(7) H(5) 108.1387 ? . . . N(1) C(7) H(6) 108.6530 ? . . . H(20) N(1) C(9) 106.4426 ? . . . N(1) C(9) H(10) 108.5233 ? . . . N(1) C(9) H(11) 108.2369 ? . . . H(20) N(1) C(11) 106.4152 ? . . . N(1) C(11) H(16) 108.6654 ? . . . N(1) C(11) H(15) 108.6552 ? . . . C(1) C(6) H(4) 119.3890 ? . . . C(2) C(3) H(1) 119.2627 ? . . . H(1) C(3) C(4) 120.7256 ? . . . C(3) C(4) H(2) 119.5579 ? . . . C(4) C(5) H(3) 120.2276 ? . . . H(2) C(4) C(5) 119.8058 ? . . . C(5) C(6) H(4) 120.3002 ? . . . H(3) C(5) C(6) 119.7884 ? . . . C(7) C(8) H(8) 110.1607 ? . . . C(7) C(8) H(7) 108.3715 ? . . . H(5) C(7) C(8) 107.5725 ? . . . H(6) C(7) C(8) 109.3494 ? . . . C(7) C(8) H(9) 109.8758 ? . . . H(6) C(7) H(5) 109.4547 ? . . . H(8) C(8) H(7) 109.4697 ? . . . H(9) C(8) H(7) 109.4691 ? . . . H(9) C(8) H(8) 109.4746 ? . . . H(10) C(9) C(10) 108.1028 ? . . . H(11) C(9) C(10) 108.3964 ? . . . C(9) C(10) H(12) 110.3627 ? . . . C(9) C(10) H(13) 108.8736 ? . . . C(9) C(10) H(14) 109.1771 ? . . . H(11) C(9) H(10) 109.4572 ? . . . H(13) C(10) H(12) 109.4650 ? . . . H(14) C(10) H(12) 109.4726 ? . . . H(14) C(10) H(13) 109.4726 ? . . . C(11) C(12) H(18) 109.7661 ? . . . H(16) C(11) C(12) 108.1292 ? . . . H(15) C(11) C(12) 108.9253 ? . . . C(11) C(12) H(17) 109.6689 ? . . . C(11) C(12) H(19) 108.9709 ? . . . H(16) C(11) H(15) 109.4560 ? . . . H(18) C(12) H(17) 109.4728 ? . . . H(19) C(12) H(17) 109.4666 ? . . . H(19) C(12) H(18) 109.4809 ? . . . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 O(1) Mo(1) S(1) C(1) -87.5(5) ? . . . . O(2) Mo(1) S(1) C(1) -1.4(6) ? . . . . S(1) Mo(1) O(2) C(2) 4.2(7) ? . . . . O(1) Mo(1) O(2) C(2) 111(1) ? . . . . Mo(1) S(1) C(1) C(2) -0.7(1) ? . . . . Mo(1) S(1) C(1) C(6) -178.6(1) ? . . . . Mo(1) O(2) C(2) C(1) -6.1(2) ? . . . . Mo(1) O(2) C(2) C(3) 174.8(1) ? . . . . C(9) N(1) C(7) C(8) 70.5(2) ? . . . . C(11) N(1) C(7) C(8) -161.4(2) ? . . . . C(7) N(1) C(9) C(10) 73.4(2) ? . . . . C(11) N(1) C(9) C(10) -52.8(2) ? . . . . C(7) N(1) C(11) C(12) 175.0(1) ? . . . . C(9) N(1) C(11) C(12) -56.1(2) ? . . . . S(1) C(1) C(2) O(2) 3.9(2) ? . . . . S(1) C(1) C(2) C(3) -177.0(1) ? . . . . C(6) C(1) C(2) O(2) -178.2(1) ? . . . . C(6) C(1) C(2) C(3) 0.9(2) ? . . . . S(1) C(1) C(6) C(5) 177.2(2) ? . . . . C(2) C(1) C(6) C(5) -0.6(3) ? . . . . O(2) C(2) C(3) C(4) 178.6(2) ? . . . . C(1) C(2) C(3) C(4) -0.5(2) ? . . . . C(2) C(3) C(4) C(5) -0.2(3) ? . . . . C(3) C(4) C(5) C(6) 0.6(3) ? . . . . C(4) C(5) C(6) C(1) -0.2(3) ? . . . . loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_publ_flag _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 O(1) N(1) 2.773(2) ? . . #============================================================================== # Additional structures and associated data_? identifiers # should be added at this point if there is more than one # structure analysis in the CIF. #============================================================================== # End of CIF