# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Sabyasachi Sarkar' _publ_contact_author_email ABYA@IITK.AC.IN _publ_section_title ; Necessity of Fine Tuning in Mo(IV) Bis(Dithiolene) Complexes to Warrant Nitrate Reduction ; loop_ _publ_author_name 'Sabyasachi Sarkar' 'Amit Majumdar' 'Kuntal Pal' #===END data_8jula _database_code_depnum_ccdc_archive 'CCDC 673220' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H15 Mo N5 P S5, C8 H20 N' _chemical_formula_sum 'C35 H35 Mo N6 P S5' _chemical_formula_weight 826.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_Int_Tables_number 33 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 25.720(5) _cell_length_b 19.829(5) _cell_length_c 15.048(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7675(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour Red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3392 _exptl_absorpt_coefficient_mu 0.689 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.919 _exptl_absorpt_correction_T_max 0.948 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49730 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0728 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 28.28 _reflns_number_total 18610 _reflns_number_gt 15596 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker)' _computing_cell_refinement 'SMART (Bruker)' _computing_data_reduction 'SAINT (Bruker)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2000)' _computing_publication_material 'SHELXTL (Bruker, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0304P)^2^+5.4079P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.0(4) _refine_ls_number_reflns 18610 _refine_ls_number_parameters 874 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.0954 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.227735(12) 0.915034(15) 0.66616(3) 0.01242(7) Uani 1 1 d . . . Mo2 Mo 0.958879(12) 0.246087(15) 0.65662(3) 0.01203(7) Uani 1 1 d . . . P1 P 0.14022(4) 0.97418(5) 0.66690(9) 0.0140(2) Uani 1 1 d . . . P2 P 0.87744(4) 0.31704(5) 0.66964(8) 0.0134(2) Uani 1 1 d . . . S1 S 0.27646(4) 0.85296(5) 0.77104(8) 0.0172(2) Uani 1 1 d . . . S2 S 0.25154(4) 1.00562(5) 0.75512(7) 0.0150(2) Uani 1 1 d . . . S3 S 0.26775(5) 0.83814(5) 0.56819(8) 0.0183(2) Uani 1 1 d . . . S4 S 0.23834(4) 0.98838(5) 0.54645(7) 0.0149(2) Uani 1 1 d . . . S5 S 0.10304(5) 0.74957(6) 0.76769(9) 0.0292(3) Uani 1 1 d . . . S6 S 0.97663(4) 0.32042(5) 0.54028(8) 0.0165(2) Uani 1 1 d . . . S7 S 0.97836(4) 0.16438(5) 0.54880(7) 0.0150(2) Uani 1 1 d . . . S8 S 0.99207(4) 0.33074(5) 0.74751(8) 0.0178(2) Uani 1 1 d . . . S9 S 1.01352(4) 0.17702(5) 0.74299(7) 0.0168(2) Uani 1 1 d . . . S10 S 0.82055(5) 0.10725(6) 0.77631(10) 0.0348(3) Uani 1 1 d . . . N1 N 0.35757(17) 0.8596(2) 0.9736(3) 0.0330(10) Uani 1 1 d . . . N2 N 0.32232(16) 1.05760(18) 0.9631(3) 0.0265(9) Uani 1 1 d . . . N3 N 0.32538(16) 0.81272(19) 0.3425(3) 0.0259(9) Uani 1 1 d . . . N4 N 0.28787(16) 1.0115(2) 0.3165(3) 0.0262(9) Uani 1 1 d . . . N5 N 0.17399(13) 0.83927(16) 0.6928(2) 0.0157(8) Uani 1 1 d . . . N6 N 1.03109(16) 0.3402(2) 0.3133(3) 0.0290(10) Uani 1 1 d . . . N7 N 1.02746(16) 0.13217(19) 0.3201(3) 0.0285(10) Uani 1 1 d . . . N8 N 1.07001(19) 0.3746(3) 0.9426(3) 0.0537(15) Uani 1 1 d . . . N9 N 1.11367(18) 0.1675(2) 0.9163(3) 0.0347(10) Uani 1 1 d . . . N10 N 0.90130(13) 0.17750(16) 0.6945(2) 0.0143(8) Uani 1 1 d . . . N11 N 0.32702(13) 0.61191(17) 0.6599(3) 0.0242(8) Uani 1 1 d . . . N12 N 0.56997(12) 0.97148(15) 0.6511(3) 0.0159(7) Uani 1 1 d . . . C1 C 0.29885(17) 0.9086(2) 0.8502(3) 0.0174(9) Uani 1 1 d . . . C2 C 0.33130(18) 0.8812(2) 0.9195(3) 0.0215(10) Uani 1 1 d . . . C3 C 0.28761(16) 0.9753(2) 0.8445(3) 0.0142(9) Uani 1 1 d . . . C4 C 0.30657(18) 1.0221(2) 0.9092(3) 0.0194(10) Uani 1 1 d . . . C5 C 0.28119(17) 0.8791(2) 0.4697(3) 0.0172(9) Uani 1 1 d . . . C6 C 0.30565(18) 0.8422(2) 0.3993(3) 0.0186(9) Uani 1 1 d . . . C7 C 0.26756(16) 0.9454(2) 0.4601(3) 0.0144(9) Uani 1 1 d . . . C8 C 0.27882(16) 0.9814(2) 0.3800(3) 0.0175(9) Uani 1 1 d . . . C9 C 0.13675(16) 1.0628(2) 0.6327(3) 0.0150(9) Uani 1 1 d . . . C10 C 0.12000(17) 1.0827(2) 0.5486(3) 0.0190(9) Uani 1 1 d . . . H10 H 0.1090 1.0507 0.5076 0.023 Uiso 1 1 calc R . . C11 C 0.11984(17) 1.1503(2) 0.5267(3) 0.0235(10) Uani 1 1 d . . . H11 H 0.1092 1.1634 0.4703 0.028 Uiso 1 1 calc R . . C12 C 0.13528(18) 1.1990(2) 0.5871(3) 0.0277(11) Uani 1 1 d . . . H12 H 0.1345 1.2445 0.5718 0.033 Uiso 1 1 calc R . . C13 C 0.15189(15) 1.17940(19) 0.6704(4) 0.0222(10) Uani 1 1 d . . . H13 H 0.1627 1.2117 0.7112 0.027 Uiso 1 1 calc R . . C14 C 0.15256(16) 1.1120(2) 0.6934(3) 0.0180(9) Uani 1 1 d . . . H14 H 0.1636 1.0992 0.7498 0.022 Uiso 1 1 calc R . . C15 C 0.10881(16) 0.97738(19) 0.7759(3) 0.0157(9) Uani 1 1 d . . . C16 C 0.06273(17) 1.0129(2) 0.7834(3) 0.0194(9) Uani 1 1 d . . . H16 H 0.0486 1.0342 0.7339 0.023 Uiso 1 1 calc R . . C17 C 0.03759(19) 1.0167(2) 0.8651(3) 0.0246(11) Uani 1 1 d . . . H17 H 0.0069 1.0411 0.8703 0.029 Uiso 1 1 calc R . . C18 C 0.0579(2) 0.9847(2) 0.9381(3) 0.0267(11) Uani 1 1 d . . . H18 H 0.0407 0.9871 0.9924 0.032 Uiso 1 1 calc R . . C19 C 0.10387(19) 0.9486(2) 0.9311(3) 0.0225(10) Uani 1 1 d . . . H19 H 0.1178 0.9273 0.9808 0.027 Uiso 1 1 calc R . . C20 C 0.12917(17) 0.9445(2) 0.8496(3) 0.0187(9) Uani 1 1 d . . . H20 H 0.1597 0.9197 0.8444 0.022 Uiso 1 1 calc R . . C21 C 0.09595(17) 0.9266(2) 0.5966(3) 0.0172(9) Uani 1 1 d . . . C22 C 0.05355(16) 0.8929(2) 0.6332(3) 0.0200(10) Uani 1 1 d . . . H22 H 0.0454 0.8992 0.6928 0.024 Uiso 1 1 calc R . . C23 C 0.02329(18) 0.8502(2) 0.5817(3) 0.0250(11) Uani 1 1 d . . . H23 H -0.0052 0.8284 0.6065 0.030 Uiso 1 1 calc R . . C24 C 0.03566(19) 0.8402(2) 0.4938(3) 0.0289(12) Uani 1 1 d . . . H24 H 0.0156 0.8111 0.4595 0.035 Uiso 1 1 calc R . . C25 C 0.07727(19) 0.8727(2) 0.4561(3) 0.0251(11) Uani 1 1 d . . . H25 H 0.0847 0.8663 0.3962 0.030 Uiso 1 1 calc R . . C26 C 0.10817(17) 0.9147(2) 0.5067(3) 0.0209(10) Uani 1 1 d . . . H26 H 0.1371 0.9352 0.4814 0.025 Uiso 1 1 calc R . . C27 C 0.14433(17) 0.8009(2) 0.7234(3) 0.0175(9) Uani 1 1 d . . . C28 C 1.04600(16) 0.2276(2) 0.8177(3) 0.0176(9) Uani 1 1 d . . . C29 C 1.08365(19) 0.1951(2) 0.8736(3) 0.0237(10) Uani 1 1 d . . . C30 C 1.03474(18) 0.2943(2) 0.8226(3) 0.0213(10) Uani 1 1 d . . . C31 C 1.05619(19) 0.3382(3) 0.8890(3) 0.0297(12) Uani 1 1 d . . . C32 C 0.99594(17) 0.2054(2) 0.4521(3) 0.0181(9) Uani 1 1 d . . . C33 C 1.01255(17) 0.1651(2) 0.3782(3) 0.0184(9) Uani 1 1 d . . . C34 C 0.99619(17) 0.2738(2) 0.4483(3) 0.0172(9) Uani 1 1 d . . . C35 C 1.01493(18) 0.3100(2) 0.3730(3) 0.0216(10) Uani 1 1 d . . . C36 C 0.83178(17) 0.2993(2) 0.5799(3) 0.0145(9) Uani 1 1 d . . . C37 C 0.83662(18) 0.2415(2) 0.5280(3) 0.0221(10) Uani 1 1 d . . . H37 H 0.8636 0.2114 0.5388 0.027 Uiso 1 1 calc R . . C38 C 0.80150(19) 0.2285(2) 0.4606(3) 0.0259(11) Uani 1 1 d . . . H38 H 0.8048 0.1895 0.4267 0.031 Uiso 1 1 calc R . . C39 C 0.76181(18) 0.2728(2) 0.4436(3) 0.0230(10) Uani 1 1 d . . . H39 H 0.7381 0.2635 0.3985 0.028 Uiso 1 1 calc R . . C40 C 0.75676(19) 0.3314(2) 0.4928(3) 0.0249(11) Uani 1 1 d . . . H40 H 0.7303 0.3619 0.4803 0.030 Uiso 1 1 calc R . . C41 C 0.79160(16) 0.3440(2) 0.5609(3) 0.0180(9) Uani 1 1 d . . . H41 H 0.7881 0.3830 0.5947 0.022 Uiso 1 1 calc R . . C42 C 0.84224(17) 0.3037(2) 0.7743(3) 0.0167(9) Uani 1 1 d . . . C43 C 0.78862(18) 0.3149(2) 0.7783(3) 0.0200(10) Uani 1 1 d . . . H43 H 0.7706 0.3274 0.7273 0.024 Uiso 1 1 calc R . . C44 C 0.7622(2) 0.3075(2) 0.8579(4) 0.0275(12) Uani 1 1 d . . . H44 H 0.7267 0.3159 0.8607 0.033 Uiso 1 1 calc R . . C45 C 0.7889(2) 0.2876(2) 0.9330(3) 0.0287(12) Uani 1 1 d . . . H45 H 0.7712 0.2826 0.9865 0.034 Uiso 1 1 calc R . . C46 C 0.8416(2) 0.2751(2) 0.9291(3) 0.0261(11) Uani 1 1 d . . . H46 H 0.8592 0.2610 0.9798 0.031 Uiso 1 1 calc R . . C47 C 0.86837(18) 0.2835(2) 0.8504(3) 0.0198(10) Uani 1 1 d . . . H47 H 0.9040 0.2755 0.8483 0.024 Uiso 1 1 calc R . . C48 C 0.88574(14) 0.40890(18) 0.6660(3) 0.0155(8) Uani 1 1 d . . . C49 C 0.89473(17) 0.4444(2) 0.7439(3) 0.0201(10) Uani 1 1 d . . . H49 H 0.8964 0.4214 0.7978 0.024 Uiso 1 1 calc R . . C50 C 0.90125(18) 0.5138(2) 0.7422(4) 0.0234(11) Uani 1 1 d . . . H50 H 0.9078 0.5372 0.7946 0.028 Uiso 1 1 calc R . . C51 C 0.89796(15) 0.54807(19) 0.6626(5) 0.0292(11) Uani 1 1 d . . . H51 H 0.9015 0.5947 0.6614 0.035 Uiso 1 1 calc R . . C52 C 0.88935(18) 0.5128(2) 0.5842(4) 0.0247(11) Uani 1 1 d . . . H52 H 0.8871 0.5361 0.5307 0.030 Uiso 1 1 calc R . . C53 C 0.88407(17) 0.4435(2) 0.5849(3) 0.0191(10) Uani 1 1 d . . . H53 H 0.8795 0.4200 0.5320 0.023 Uiso 1 1 calc R . . C54 C 0.86713(17) 0.1477(2) 0.7272(3) 0.0203(10) Uani 1 1 d . . . C55 C 0.62141(15) 1.00919(19) 0.6516(3) 0.0170(9) Uani 1 1 d . . . H55A H 0.6459 0.9841 0.6878 0.020 Uiso 1 1 calc R . . H55B H 0.6349 1.0101 0.5915 0.020 Uiso 1 1 calc R . . C56 C 0.61912(19) 1.0810(2) 0.6860(3) 0.0301(12) Uani 1 1 d . . . H56A H 0.5941 1.1061 0.6523 0.045 Uiso 1 1 calc R . . H56B H 0.6527 1.1016 0.6801 0.045 Uiso 1 1 calc R . . H56C H 0.6091 1.0807 0.7475 0.045 Uiso 1 1 calc R . . C57 C 0.53116(18) 1.0055(2) 0.5901(3) 0.0219(10) Uani 1 1 d . . . H57A H 0.4981 0.9823 0.5953 0.026 Uiso 1 1 calc R . . H57B H 0.5260 1.0514 0.6106 0.026 Uiso 1 1 calc R . . C58 C 0.54634(19) 1.0076(2) 0.4931(3) 0.0286(11) Uani 1 1 d . . . H58A H 0.5784 1.0319 0.4866 0.043 Uiso 1 1 calc R . . H58B H 0.5196 1.0298 0.4596 0.043 Uiso 1 1 calc R . . H58C H 0.5507 0.9624 0.4714 0.043 Uiso 1 1 calc R . . C59 C 0.54573(17) 0.9710(2) 0.7432(3) 0.0202(10) Uani 1 1 d . . . H59A H 0.5357 1.0168 0.7581 0.024 Uiso 1 1 calc R . . H59B H 0.5142 0.9442 0.7409 0.024 Uiso 1 1 calc R . . C60 C 0.57966(19) 0.9441(2) 0.8168(3) 0.0267(11) Uani 1 1 d . . . H60A H 0.5896 0.8985 0.8034 0.040 Uiso 1 1 calc R . . H60B H 0.5607 0.9449 0.8718 0.040 Uiso 1 1 calc R . . H60C H 0.6102 0.9716 0.8221 0.040 Uiso 1 1 calc R . . C61 C 0.58224(17) 0.8999(2) 0.6203(3) 0.0201(10) Uani 1 1 d . . . H61A H 0.6020 0.9026 0.5655 0.024 Uiso 1 1 calc R . . H61B H 0.6042 0.8786 0.6645 0.024 Uiso 1 1 calc R . . C62 C 0.5355(2) 0.8552(2) 0.6045(3) 0.0296(12) Uani 1 1 d . . . H62A H 0.5144 0.8541 0.6572 0.044 Uiso 1 1 calc R . . H62B H 0.5469 0.8104 0.5905 0.044 Uiso 1 1 calc R . . H62C H 0.5155 0.8728 0.5560 0.044 Uiso 1 1 calc R . . C63 C 0.3538(2) 0.6761(2) 0.6268(3) 0.0358(13) Uani 1 1 d . . . H63A H 0.3810 0.6630 0.5857 0.043 Uiso 1 1 calc R . . H63B H 0.3285 0.7021 0.5934 0.043 Uiso 1 1 calc R . . C64 C 0.3775(2) 0.7219(2) 0.6957(4) 0.0373(14) Uani 1 1 d . . . H64A H 0.3518 0.7328 0.7398 0.056 Uiso 1 1 calc R . . H64B H 0.3894 0.7626 0.6677 0.056 Uiso 1 1 calc R . . H64C H 0.4063 0.6995 0.7235 0.056 Uiso 1 1 calc R . . C65 C 0.28305(19) 0.6282(3) 0.7221(3) 0.0310(12) Uani 1 1 d . . . H65A H 0.2967 0.6549 0.7708 0.037 Uiso 1 1 calc R . . H65B H 0.2701 0.5864 0.7470 0.037 Uiso 1 1 calc R . . C66 C 0.2370(2) 0.6665(2) 0.6810(4) 0.0389(14) Uani 1 1 d . . . H66A H 0.2490 0.7088 0.6575 0.058 Uiso 1 1 calc R . . H66B H 0.2112 0.6746 0.7257 0.058 Uiso 1 1 calc R . . H66C H 0.2222 0.6401 0.6339 0.058 Uiso 1 1 calc R . . C67 C 0.3086(2) 0.5741(3) 0.5771(4) 0.0358(13) Uani 1 1 d . . . H67A H 0.2849 0.6030 0.5445 0.043 Uiso 1 1 calc R . . H67B H 0.3384 0.5657 0.5392 0.043 Uiso 1 1 calc R . . C68 C 0.2816(2) 0.5075(3) 0.5953(4) 0.0455(15) Uani 1 1 d . . . H68A H 0.3038 0.4795 0.6311 0.068 Uiso 1 1 calc R . . H68B H 0.2744 0.4852 0.5401 0.068 Uiso 1 1 calc R . . H68C H 0.2496 0.5157 0.6264 0.068 Uiso 1 1 calc R . . C69 C 0.3653(2) 0.5694(2) 0.7139(3) 0.0311(12) Uani 1 1 d . . . H69A H 0.3792 0.5973 0.7612 0.037 Uiso 1 1 calc R . . H69B H 0.3461 0.5329 0.7416 0.037 Uiso 1 1 calc R . . C70 C 0.41043(18) 0.5392(3) 0.6632(5) 0.0418(13) Uani 1 1 d . . . H70A H 0.3975 0.5077 0.6202 0.063 Uiso 1 1 calc R . . H70B H 0.4332 0.5164 0.7039 0.063 Uiso 1 1 calc R . . H70C H 0.4292 0.5745 0.6335 0.063 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.01455(16) 0.01019(14) 0.01253(16) 0.00043(15) -0.00064(17) -0.00090(12) Mo2 0.01365(15) 0.00960(14) 0.01285(16) -0.00068(15) 0.00055(17) -0.00019(12) P1 0.0166(5) 0.0114(4) 0.0141(5) 0.0003(5) -0.0013(5) 0.0001(4) P2 0.0154(5) 0.0101(4) 0.0146(5) -0.0019(5) 0.0005(5) -0.0006(4) S1 0.0226(6) 0.0121(5) 0.0169(6) 0.0019(4) -0.0032(5) 0.0001(4) S2 0.0181(5) 0.0107(5) 0.0162(6) 0.0001(4) -0.0034(4) -0.0005(4) S3 0.0268(6) 0.0111(5) 0.0171(6) -0.0001(4) 0.0017(5) 0.0005(4) S4 0.0175(5) 0.0111(5) 0.0161(6) 0.0010(4) 0.0004(4) 0.0002(4) S5 0.0273(6) 0.0204(6) 0.0398(8) 0.0035(5) 0.0079(6) -0.0071(5) S6 0.0203(6) 0.0105(5) 0.0187(6) 0.0010(4) 0.0022(4) 0.0007(4) S7 0.0185(5) 0.0109(5) 0.0156(6) -0.0014(4) 0.0014(4) 0.0003(4) S8 0.0191(6) 0.0139(5) 0.0205(6) -0.0048(4) 0.0003(5) -0.0019(4) S9 0.0193(6) 0.0148(5) 0.0164(6) 0.0010(4) -0.0038(4) 0.0004(4) S10 0.0327(7) 0.0250(6) 0.0467(9) -0.0047(6) 0.0163(6) -0.0134(5) N1 0.046(3) 0.025(2) 0.028(2) 0.0091(19) -0.016(2) -0.006(2) N2 0.039(3) 0.021(2) 0.020(2) 0.0006(17) -0.0117(18) -0.0007(19) N3 0.032(2) 0.019(2) 0.026(2) 0.0008(17) 0.0048(18) -0.0027(17) N4 0.027(2) 0.029(2) 0.023(2) 0.0070(18) 0.0023(18) 0.0032(18) N5 0.0154(18) 0.0127(17) 0.019(2) 0.0022(14) -0.0011(14) 0.0011(14) N6 0.032(2) 0.027(2) 0.027(2) 0.0069(19) 0.0003(19) 0.0014(19) N7 0.035(2) 0.028(2) 0.023(2) -0.0076(18) 0.0057(19) -0.0016(19) N8 0.037(3) 0.075(4) 0.049(3) -0.038(3) 0.002(2) -0.012(3) N9 0.036(3) 0.043(3) 0.025(2) 0.007(2) -0.010(2) -0.003(2) N10 0.0139(18) 0.0110(16) 0.018(2) 0.0000(13) 0.0029(14) -0.0043(14) N11 0.0242(19) 0.0290(18) 0.0193(19) 0.006(2) -0.002(2) -0.0018(15) N12 0.0159(17) 0.0158(16) 0.016(2) -0.0003(16) 0.0001(16) 0.0032(13) C1 0.020(2) 0.022(2) 0.011(2) -0.0016(18) -0.0013(18) -0.0040(19) C2 0.024(3) 0.015(2) 0.025(3) 0.0030(19) -0.005(2) -0.0081(19) C3 0.014(2) 0.014(2) 0.014(2) 0.0004(16) -0.0019(17) -0.0022(17) C4 0.023(2) 0.017(2) 0.018(2) 0.0048(18) -0.0005(19) 0.0017(18) C5 0.015(2) 0.018(2) 0.019(2) -0.0026(18) 0.0013(18) -0.0027(17) C6 0.024(2) 0.019(2) 0.012(2) 0.0019(17) 0.0031(18) -0.0012(19) C7 0.015(2) 0.016(2) 0.012(2) 0.0038(17) -0.0028(17) -0.0045(17) C8 0.011(2) 0.020(2) 0.022(2) -0.0030(19) 0.0026(17) 0.0012(17) C9 0.013(2) 0.017(2) 0.015(2) 0.0029(16) 0.0025(16) 0.0025(16) C10 0.022(2) 0.019(2) 0.016(2) 0.0051(18) -0.0014(18) -0.0009(18) C11 0.023(2) 0.029(2) 0.019(3) 0.012(2) -0.0022(19) 0.001(2) C12 0.022(3) 0.019(2) 0.042(3) 0.008(2) 0.008(2) 0.0040(19) C13 0.019(2) 0.0126(18) 0.035(3) 0.002(2) 0.001(2) -0.0019(15) C14 0.018(2) 0.018(2) 0.018(2) -0.0007(17) 0.0009(17) 0.0025(17) C15 0.024(2) 0.0128(19) 0.010(2) -0.0010(16) 0.0007(18) -0.0060(17) C16 0.025(2) 0.013(2) 0.020(2) -0.0009(18) 0.0029(19) -0.0024(18) C17 0.033(3) 0.013(2) 0.027(3) -0.0049(19) 0.014(2) -0.005(2) C18 0.042(3) 0.017(2) 0.020(3) -0.0034(19) 0.009(2) -0.010(2) C19 0.034(3) 0.018(2) 0.015(2) -0.0028(18) 0.000(2) -0.007(2) C20 0.016(2) 0.016(2) 0.024(2) 0.0011(18) 0.0034(19) -0.0018(18) C21 0.018(2) 0.016(2) 0.018(2) 0.0024(17) -0.0027(17) 0.0015(18) C22 0.017(2) 0.024(2) 0.019(2) -0.0040(18) -0.0017(17) -0.0016(18) C23 0.019(2) 0.024(2) 0.033(3) -0.002(2) -0.006(2) -0.0036(19) C24 0.027(3) 0.029(3) 0.031(3) -0.008(2) -0.013(2) 0.002(2) C25 0.029(3) 0.027(2) 0.018(3) -0.007(2) -0.009(2) 0.008(2) C26 0.016(2) 0.024(2) 0.023(3) -0.0027(19) 0.0000(19) 0.0013(19) C27 0.021(2) 0.016(2) 0.015(2) -0.0050(17) -0.0046(18) 0.0035(18) C28 0.011(2) 0.028(2) 0.014(2) -0.0024(18) 0.0022(17) -0.0017(18) C29 0.026(3) 0.032(3) 0.013(2) 0.002(2) 0.001(2) -0.005(2) C30 0.022(2) 0.024(2) 0.018(2) -0.0040(19) 0.0009(19) -0.0035(19) C31 0.027(3) 0.036(3) 0.027(3) -0.011(2) 0.001(2) -0.003(2) C32 0.016(2) 0.020(2) 0.018(2) -0.0039(18) -0.0032(18) 0.0004(18) C33 0.024(2) 0.015(2) 0.016(2) 0.0024(18) -0.0029(19) -0.0079(18) C34 0.017(2) 0.022(2) 0.013(2) 0.0030(17) -0.0023(17) 0.0019(18) C35 0.026(3) 0.021(2) 0.018(3) -0.0042(19) -0.003(2) 0.0038(19) C36 0.016(2) 0.0131(19) 0.014(2) -0.0024(17) 0.0027(17) -0.0046(17) C37 0.026(2) 0.021(2) 0.020(2) -0.0012(19) -0.0070(19) 0.0110(19) C38 0.032(3) 0.020(2) 0.025(3) -0.008(2) -0.005(2) 0.001(2) C39 0.024(3) 0.020(2) 0.025(3) -0.0029(19) -0.010(2) 0.002(2) C40 0.020(3) 0.019(2) 0.036(3) 0.002(2) -0.003(2) 0.005(2) C41 0.019(2) 0.015(2) 0.021(2) -0.0060(18) -0.0006(19) 0.0038(17) C42 0.023(2) 0.0128(19) 0.015(2) -0.0011(17) 0.0039(19) -0.0056(17) C43 0.026(2) 0.012(2) 0.022(2) -0.0018(18) 0.006(2) -0.0026(18) C44 0.026(3) 0.015(2) 0.041(3) -0.006(2) 0.017(2) -0.002(2) C45 0.041(3) 0.017(2) 0.027(3) 0.000(2) 0.016(2) -0.008(2) C46 0.043(3) 0.019(2) 0.016(2) 0.0011(19) 0.005(2) -0.002(2) C47 0.023(2) 0.017(2) 0.020(2) 0.0019(18) 0.0037(19) 0.0002(18) C48 0.0148(18) 0.0141(17) 0.018(2) 0.004(2) 0.008(2) 0.0025(14) C49 0.017(2) 0.019(2) 0.025(3) -0.004(2) 0.008(2) -0.0002(18) C50 0.018(2) 0.021(2) 0.032(3) -0.009(2) 0.002(2) -0.0043(19) C51 0.018(2) 0.0099(18) 0.060(3) -0.004(3) 0.001(3) -0.0011(15) C52 0.015(2) 0.015(2) 0.044(3) 0.014(2) 0.001(2) 0.0010(18) C53 0.010(2) 0.020(2) 0.028(3) 0.001(2) -0.0013(19) 0.0010(18) C54 0.024(3) 0.014(2) 0.024(3) -0.0047(18) -0.0033(19) 0.0029(18) C55 0.0133(19) 0.024(2) 0.014(2) -0.0015(19) 0.0019(18) -0.0006(16) C56 0.037(3) 0.030(3) 0.024(3) -0.004(2) 0.006(2) -0.008(2) C57 0.022(2) 0.025(2) 0.020(3) 0.0040(19) -0.0041(19) 0.005(2) C58 0.028(3) 0.038(3) 0.019(3) 0.007(2) -0.007(2) 0.000(2) C59 0.024(2) 0.018(2) 0.019(2) 0.0017(18) 0.005(2) 0.0015(18) C60 0.028(3) 0.034(3) 0.018(3) 0.000(2) 0.003(2) 0.000(2) C61 0.025(2) 0.018(2) 0.017(2) 0.0012(18) 0.0030(19) 0.0006(19) C62 0.038(3) 0.023(2) 0.028(3) -0.004(2) -0.002(2) -0.007(2) C63 0.045(3) 0.028(3) 0.035(3) 0.004(2) 0.013(3) -0.010(2) C64 0.038(3) 0.024(3) 0.050(4) -0.002(2) 0.000(3) 0.000(2) C65 0.030(3) 0.035(3) 0.027(3) 0.006(2) 0.002(2) -0.002(2) C66 0.041(3) 0.030(3) 0.046(4) 0.009(3) 0.005(3) 0.012(2) C67 0.033(3) 0.039(3) 0.035(3) 0.007(2) -0.003(2) -0.003(2) C68 0.055(4) 0.041(3) 0.041(4) 0.002(3) -0.014(3) -0.009(3) C69 0.035(3) 0.028(3) 0.030(3) 0.002(2) -0.009(2) 0.004(2) C70 0.031(3) 0.048(3) 0.046(3) -0.019(3) -0.008(3) 0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 N5 2.080(3) . ? Mo1 S2 2.3225(12) . ? Mo1 S4 2.3311(12) . ? Mo1 S3 2.3574(12) . ? Mo1 S1 2.3614(12) . ? Mo1 P1 2.5380(11) . ? Mo2 N10 2.090(3) . ? Mo2 S8 2.3275(12) . ? Mo2 S6 2.3337(12) . ? Mo2 S7 2.3470(12) . ? Mo2 S9 2.3536(12) . ? Mo2 P2 2.5308(11) . ? P1 C21 1.819(4) . ? P1 C15 1.829(4) . ? P1 C9 1.833(4) . ? P2 C36 1.824(4) . ? P2 C48 1.835(4) . ? P2 C42 1.836(5) . ? S1 C1 1.723(4) . ? S2 C3 1.741(4) . ? S3 C5 1.725(5) . ? S4 C7 1.726(4) . ? S5 C27 1.615(5) . ? S6 C34 1.739(4) . ? S7 C32 1.728(5) . ? S8 C30 1.733(5) . ? S9 C28 1.723(4) . ? S10 C54 1.621(5) . ? N1 C2 1.142(6) . ? N2 C4 1.148(6) . ? N3 C6 1.154(5) . ? N4 C8 1.151(6) . ? N5 C27 1.172(5) . ? N6 C35 1.157(6) . ? N7 C33 1.157(6) . ? N8 C31 1.138(6) . ? N9 C29 1.145(6) . ? N10 C54 1.167(5) . ? N11 C65 1.503(6) . ? N11 C69 1.529(6) . ? N11 C67 1.530(7) . ? N11 C63 1.531(6) . ? N12 C57 1.515(5) . ? N12 C59 1.520(6) . ? N12 C55 1.520(5) . ? N12 C61 1.526(5) . ? C1 C3 1.357(6) . ? C1 C2 1.441(6) . ? C3 C4 1.430(6) . ? C5 C7 1.369(6) . ? C5 C6 1.433(6) . ? C7 C8 1.430(6) . ? C9 C10 1.393(6) . ? C9 C14 1.398(5) . ? C10 C11 1.381(6) . ? C10 H10 0.9300 . ? C11 C12 1.385(7) . ? C11 H11 0.9300 . ? C12 C13 1.380(7) . ? C12 H12 0.9300 . ? C13 C14 1.381(5) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.383(6) . ? C15 C20 1.390(6) . ? C16 C17 1.392(6) . ? C16 H16 0.9300 . ? C17 C18 1.372(7) . ? C17 H17 0.9300 . ? C18 C19 1.387(7) . ? C18 H18 0.9300 . ? C19 C20 1.391(6) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.392(6) . ? C21 C26 1.408(6) . ? C22 C23 1.387(6) . ? C22 H22 0.9300 . ? C23 C24 1.375(7) . ? C23 H23 0.9300 . ? C24 C25 1.372(7) . ? C24 H24 0.9300 . ? C25 C26 1.381(6) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C28 C30 1.356(6) . ? C28 C29 1.435(6) . ? C30 C31 1.435(6) . ? C32 C34 1.357(6) . ? C32 C33 1.434(6) . ? C34 C35 1.425(6) . ? C36 C41 1.390(6) . ? C36 C37 1.393(6) . ? C37 C38 1.382(6) . ? C37 H37 0.9300 . ? C38 C39 1.372(6) . ? C38 H38 0.9300 . ? C39 C40 1.383(6) . ? C39 H39 0.9300 . ? C40 C41 1.385(6) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C47 1.386(6) . ? C42 C43 1.398(6) . ? C43 C44 1.384(6) . ? C43 H43 0.9300 . ? C44 C45 1.379(7) . ? C44 H44 0.9300 . ? C45 C46 1.380(7) . ? C45 H45 0.9300 . ? C46 C47 1.381(6) . ? C46 H46 0.9300 . ? C47 H47 0.9300 . ? C48 C49 1.387(7) . ? C48 C53 1.401(6) . ? C49 C50 1.386(6) . ? C49 H49 0.9300 . ? C50 C51 1.381(8) . ? C50 H50 0.9300 . ? C51 C52 1.388(8) . ? C51 H51 0.9300 . ? C52 C53 1.381(6) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C55 C56 1.516(6) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C58 1.512(6) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 C60 1.508(6) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 C62 1.512(6) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C63 C64 1.506(7) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? C65 C66 1.536(7) . ? C65 H65A 0.9700 . ? C65 H65B 0.9700 . ? C66 H66A 0.9600 . ? C66 H66B 0.9600 . ? C66 H66C 0.9600 . ? C67 C68 1.517(7) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? C69 C70 1.512(7) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Mo1 S2 128.52(10) . . ? N5 Mo1 S4 132.61(10) . . ? S2 Mo1 S4 86.10(5) . . ? N5 Mo1 S3 86.75(10) . . ? S2 Mo1 S3 138.21(4) . . ? S4 Mo1 S3 82.48(4) . . ? N5 Mo1 S1 81.23(10) . . ? S2 Mo1 S1 82.99(4) . . ? S4 Mo1 S1 141.22(4) . . ? S3 Mo1 S1 81.32(4) . . ? N5 Mo1 P1 75.15(10) . . ? S2 Mo1 P1 82.75(4) . . ? S4 Mo1 P1 79.57(4) . . ? S3 Mo1 P1 133.54(4) . . ? S1 Mo1 P1 135.11(5) . . ? N10 Mo2 S8 124.66(10) . . ? N10 Mo2 S6 138.98(10) . . ? S8 Mo2 S6 85.04(5) . . ? N10 Mo2 S7 83.73(9) . . ? S8 Mo2 S7 145.67(4) . . ? S6 Mo2 S7 82.86(4) . . ? N10 Mo2 S9 83.89(10) . . ? S8 Mo2 S9 82.89(4) . . ? S6 Mo2 S9 131.68(4) . . ? S7 Mo2 S9 81.52(4) . . ? N10 Mo2 P2 75.77(10) . . ? S8 Mo2 P2 81.79(4) . . ? S6 Mo2 P2 82.46(4) . . ? S7 Mo2 P2 127.87(4) . . ? S9 Mo2 P2 140.80(4) . . ? C21 P1 C15 105.3(2) . . ? C21 P1 C9 107.66(19) . . ? C15 P1 C9 101.37(18) . . ? C21 P1 Mo1 108.23(14) . . ? C15 P1 Mo1 114.31(14) . . ? C9 P1 Mo1 119.00(14) . . ? C36 P2 C48 104.1(2) . . ? C36 P2 C42 106.9(2) . . ? C48 P2 C42 103.0(2) . . ? C36 P2 Mo2 111.62(14) . . ? C48 P2 Mo2 116.96(12) . . ? C42 P2 Mo2 113.24(15) . . ? C1 S1 Mo1 107.83(16) . . ? C3 S2 Mo1 108.60(14) . . ? C5 S3 Mo1 108.67(15) . . ? C7 S4 Mo1 108.96(14) . . ? C34 S6 Mo2 108.55(15) . . ? C32 S7 Mo2 108.26(15) . . ? C30 S8 Mo2 108.37(15) . . ? C28 S9 Mo2 108.10(16) . . ? C27 N5 Mo1 167.7(3) . . ? C54 N10 Mo2 167.8(3) . . ? C65 N11 C69 105.8(4) . . ? C65 N11 C67 112.3(4) . . ? C69 N11 C67 111.2(4) . . ? C65 N11 C63 111.2(4) . . ? C69 N11 C63 110.0(4) . . ? C67 N11 C63 106.4(4) . . ? C57 N12 C59 106.5(3) . . ? C57 N12 C55 111.0(3) . . ? C59 N12 C55 110.8(3) . . ? C57 N12 C61 111.5(3) . . ? C59 N12 C61 110.9(3) . . ? C55 N12 C61 106.2(3) . . ? C3 C1 C2 122.4(4) . . ? C3 C1 S1 120.6(3) . . ? C2 C1 S1 117.0(3) . . ? N1 C2 C1 179.1(6) . . ? C1 C3 C4 121.1(4) . . ? C1 C3 S2 119.9(3) . . ? C4 C3 S2 118.9(3) . . ? N2 C4 C3 177.4(5) . . ? C7 C5 C6 121.6(4) . . ? C7 C5 S3 119.5(3) . . ? C6 C5 S3 118.9(3) . . ? N3 C6 C5 179.8(6) . . ? C5 C7 C8 121.1(4) . . ? C5 C7 S4 120.4(3) . . ? C8 C7 S4 118.5(3) . . ? N4 C8 C7 178.7(5) . . ? C10 C9 C14 119.1(4) . . ? C10 C9 P1 122.8(3) . . ? C14 C9 P1 118.1(3) . . ? C11 C10 C9 119.5(4) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 121.3(4) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C13 C12 C11 119.2(4) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 120.3(4) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C13 C14 C9 120.5(4) . . ? C13 C14 H14 119.7 . . ? C9 C14 H14 119.7 . . ? C16 C15 C20 119.8(4) . . ? C16 C15 P1 118.0(3) . . ? C20 C15 P1 122.2(3) . . ? C15 C16 C17 119.9(4) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 120.4(5) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 120.2(4) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C18 C19 C20 119.8(4) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C15 C20 C19 120.0(4) . . ? C15 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C26 118.3(4) . . ? C22 C21 P1 120.6(3) . . ? C26 C21 P1 120.4(3) . . ? C23 C22 C21 120.8(4) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C24 C23 C22 119.7(5) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C25 C24 C23 120.7(4) . . ? C25 C24 H24 119.6 . . ? C23 C24 H24 119.6 . . ? C24 C25 C26 120.3(5) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 120.1(4) . . ? C25 C26 H26 119.9 . . ? C21 C26 H26 119.9 . . ? N5 C27 S5 178.4(4) . . ? C30 C28 C29 123.4(4) . . ? C30 C28 S9 120.0(4) . . ? C29 C28 S9 116.6(3) . . ? N9 C29 C28 177.8(5) . . ? C28 C30 C31 123.2(4) . . ? C28 C30 S8 120.4(3) . . ? C31 C30 S8 116.4(4) . . ? N8 C31 C30 175.5(6) . . ? C34 C32 C33 121.5(4) . . ? C34 C32 S7 120.4(3) . . ? C33 C32 S7 117.9(3) . . ? N7 C33 C32 177.7(5) . . ? C32 C34 C35 122.5(4) . . ? C32 C34 S6 119.8(3) . . ? C35 C34 S6 117.6(3) . . ? N6 C35 C34 178.2(5) . . ? C41 C36 C37 118.4(4) . . ? C41 C36 P2 120.5(3) . . ? C37 C36 P2 121.1(3) . . ? C38 C37 C36 120.4(4) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C39 C38 C37 120.3(4) . . ? C39 C38 H38 119.9 . . ? C37 C38 H38 119.9 . . ? C38 C39 C40 120.5(4) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C39 C40 C41 119.2(4) . . ? C39 C40 H40 120.4 . . ? C41 C40 H40 120.4 . . ? C40 C41 C36 121.2(4) . . ? C40 C41 H41 119.4 . . ? C36 C41 H41 119.4 . . ? C47 C42 C43 119.2(4) . . ? C47 C42 P2 120.7(3) . . ? C43 C42 P2 120.0(4) . . ? C44 C43 C42 120.3(5) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C45 C44 C43 119.7(5) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C45 C46 120.3(5) . . ? C44 C45 H45 119.8 . . ? C46 C45 H45 119.8 . . ? C45 C46 C47 120.3(5) . . ? C45 C46 H46 119.8 . . ? C47 C46 H46 119.8 . . ? C46 C47 C42 120.1(4) . . ? C46 C47 H47 120.0 . . ? C42 C47 H47 120.0 . . ? C49 C48 C53 119.5(3) . . ? C49 C48 P2 119.9(4) . . ? C53 C48 P2 120.6(4) . . ? C50 C49 C48 120.5(5) . . ? C50 C49 H49 119.7 . . ? C48 C49 H49 119.7 . . ? C51 C50 C49 119.8(5) . . ? C51 C50 H50 120.1 . . ? C49 C50 H50 120.1 . . ? C50 C51 C52 119.9(4) . . ? C50 C51 H51 120.0 . . ? C52 C51 H51 120.0 . . ? C53 C52 C51 120.7(5) . . ? C53 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? C52 C53 C48 119.4(5) . . ? C52 C53 H53 120.3 . . ? C48 C53 H53 120.3 . . ? N10 C54 S10 177.8(4) . . ? C56 C55 N12 115.5(3) . . ? C56 C55 H55A 108.4 . . ? N12 C55 H55A 108.4 . . ? C56 C55 H55B 108.4 . . ? N12 C55 H55B 108.4 . . ? H55A C55 H55B 107.5 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 N12 115.3(4) . . ? C58 C57 H57A 108.5 . . ? N12 C57 H57A 108.5 . . ? C58 C57 H57B 108.5 . . ? N12 C57 H57B 108.5 . . ? H57A C57 H57B 107.5 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 N12 115.8(4) . . ? C60 C59 H59A 108.3 . . ? N12 C59 H59A 108.3 . . ? C60 C59 H59B 108.3 . . ? N12 C59 H59B 108.3 . . ? H59A C59 H59B 107.4 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 N12 115.4(4) . . ? C62 C61 H61A 108.4 . . ? N12 C61 H61A 108.4 . . ? C62 C61 H61B 108.4 . . ? N12 C61 H61B 108.4 . . ? H61A C61 H61B 107.5 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 N11 117.3(4) . . ? C64 C63 H63A 108.0 . . ? N11 C63 H63A 108.0 . . ? C64 C63 H63B 108.0 . . ? N11 C63 H63B 108.0 . . ? H63A C63 H63B 107.2 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N11 C65 C66 115.8(4) . . ? N11 C65 H65A 108.3 . . ? C66 C65 H65A 108.3 . . ? N11 C65 H65B 108.3 . . ? C66 C65 H65B 108.3 . . ? H65A C65 H65B 107.4 . . ? C65 C66 H66A 109.5 . . ? C65 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C65 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C68 C67 N11 114.9(4) . . ? C68 C67 H67A 108.5 . . ? N11 C67 H67A 108.5 . . ? C68 C67 H67B 108.5 . . ? N11 C67 H67B 108.5 . . ? H67A C67 H67B 107.5 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C70 C69 N11 116.4(5) . . ? C70 C69 H69A 108.2 . . ? N11 C69 H69A 108.2 . . ? C70 C69 H69B 108.2 . . ? N11 C69 H69B 108.2 . . ? H69A C69 H69B 107.3 . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.034 _refine_diff_density_min -0.990 _refine_diff_density_rms 0.110 _ccdc_chemical_compound_source_recrystallisation 'Dichloromethane, petroleum ether' _chemical_compound_source 'Sodium Molybdate' _exptl_crystal_recrystallization_method 'Dichloromethane,petroleum ether' #===END data_8julc _database_code_depnum_ccdc_archive 'CCDC 673221' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C8 H20 N), C10 Mo N6 S6' _chemical_formula_sum 'C26 H40 Mo N8 S6' _chemical_formula_weight 753.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.857(5) _cell_length_b 15.812(5) _cell_length_c 22.444(5) _cell_angle_alpha 90.00 _cell_angle_beta 121.891(13) _cell_angle_gamma 90.00 _cell_volume 3573(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour Violet _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1560 _exptl_absorpt_coefficient_mu 0.747 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8652 _exptl_absorpt_correction_T_max 0.9428 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method /w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19692 _diffrn_reflns_av_R_equivalents 0.0929 _diffrn_reflns_av_sigmaI/netI 0.1729 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.28 _reflns_number_total 7680 _reflns_number_gt 4258 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628 (Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45 ( Bruker, 2003)' _computing_data_reduction 'SAINT 6.45 (Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e, Ortep' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1202P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0058(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7680 _refine_ls_number_parameters 407 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.1470 _refine_ls_R_factor_gt 0.0923 _refine_ls_wR_factor_ref 0.2443 _refine_ls_wR_factor_gt 0.2085 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.977 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo -0.83783(7) 0.23500(3) -0.33089(4) 0.0252(2) Uani 1 1 d . . . S1 S -0.9370(2) 0.31641(10) -0.28852(13) 0.0313(6) Uani 1 1 d . . . S2 S -0.6661(2) 0.32379(10) -0.27990(14) 0.0349(6) Uani 1 1 d . . . S3 S -0.8936(2) 0.15354(10) -0.26361(14) 0.0324(6) Uani 1 1 d . . . S4 S -0.6405(2) 0.16092(10) -0.27311(13) 0.0327(6) Uani 1 1 d . . . S5 S -1.3027(2) 0.20948(12) -0.59867(14) 0.0341(6) Uani 1 1 d . . . S6 S -0.8799(3) 0.22258(12) -0.59499(14) 0.0374(6) Uani 1 1 d . . . N1 N -0.8857(9) 0.4923(4) -0.1822(5) 0.057(3) Uani 1 1 d . . . N2 N -0.5519(9) 0.5034(4) -0.1801(5) 0.057(3) Uani 1 1 d . . . N3 N -0.7818(9) -0.0116(4) -0.1303(5) 0.053(3) Uani 1 1 d . . . N4 N -0.4589(8) -0.0026(4) -0.1481(6) 0.058(3) Uani 1 1 d . . . N5 N -1.0490(7) 0.2204(4) -0.4368(5) 0.0344(19) Uani 1 1 d . . . N6 N -0.8299(7) 0.2342(4) -0.4364(4) 0.0331(18) Uani 1 1 d . . . N7 N 0.0000 0.0000 0.0000 0.032(3) Uani 1 2 d SD . . N8 N -0.6073(7) 0.7249(3) -0.1082(4) 0.0324(18) Uani 1 1 d . . . N9 N -1.0000 0.0000 -0.5000 0.043(3) Uani 1 2 d SD . . C1 C -0.8601(9) 0.4454(4) -0.2098(5) 0.036(2) Uani 1 1 d . . . C2 C -0.8256(8) 0.3888(4) -0.2434(5) 0.032(2) Uani 1 1 d . . . C3 C -0.7086(8) 0.3922(4) -0.2405(5) 0.032(2) Uani 1 1 d . . . C4 C -0.6191(9) 0.4539(4) -0.2064(6) 0.040(3) Uani 1 1 d . . . C5 C -0.7769(9) 0.0344(5) -0.1686(5) 0.037(2) Uani 1 1 d . . . C6 C -0.7659(8) 0.0893(4) -0.2145(5) 0.0258(19) Uani 1 1 d . . . C7 C -0.6542(8) 0.0925(4) -0.2191(5) 0.033(2) Uani 1 1 d . . . C8 C -0.5446(8) 0.0402(4) -0.1789(6) 0.040(3) Uani 1 1 d . . . C9 C -1.1537(8) 0.2167(4) -0.5063(5) 0.032(2) Uani 1 1 d . . . C10 C -0.8539(8) 0.2294(4) -0.5039(5) 0.029(2) Uani 1 1 d . . . C11B C -0.1238(14) -0.0515(7) -0.0493(8) 0.033(3) Uani 0.513(11) 1 d PD A 1 H11A H -0.1060 -0.0960 -0.0730 0.040 Uiso 0.513(11) 1 calc PR A 1 H11B H -0.1964 -0.0164 -0.0835 0.040 Uiso 0.513(11) 1 calc PR A 1 C11A C -0.0245(15) -0.0340(7) 0.0601(8) 0.033(3) Uani 0.487(11) 1 d PD A 2 H11C H 0.0489 -0.0678 0.0952 0.040 Uiso 0.487(11) 1 calc PR A 2 H11D H -0.0436 0.0114 0.0825 0.040 Uiso 0.487(11) 1 calc PR A 2 C12 C -0.1502(10) -0.0887(5) 0.0105(7) 0.071(4) Uani 1 1 d D . . H12A H -0.2275 -0.1242 -0.0115 0.107 Uiso 0.487(11) 1 calc PR A 1 H12B H -0.1641 -0.0425 0.0337 0.107 Uiso 0.487(11) 1 calc PR A 1 H12C H -0.0746 -0.1210 0.0442 0.107 Uiso 0.487(11) 1 calc PR A 1 H12D H -0.1816 -0.1154 0.0374 0.107 Uiso 0.513(11) 1 d PR A 2 H12E H -0.1276 -0.1312 -0.0120 0.107 Uiso 0.513(11) 1 d PR A 2 H12F H -0.2186 -0.0529 -0.0245 0.107 Uiso 0.513(11) 1 d PR A 2 C13A C -0.1295(14) 0.0385(7) -0.0678(8) 0.044(6) Uani 0.534(15) 1 d PD A 2 H13A H -0.1093 0.0669 -0.0994 0.052 Uiso 0.534(15) 1 calc PR A 2 H13B H -0.1986 -0.0034 -0.0932 0.052 Uiso 0.534(15) 1 calc PR A 2 C13B C -0.0340(18) 0.0570(9) 0.0413(8) 0.039(6) Uani 0.466(15) 1 d PD A 1 H13C H 0.0362 0.0971 0.0696 0.046 Uiso 0.466(15) 1 calc PR A 1 H13D H -0.0572 0.0259 0.0706 0.046 Uiso 0.466(15) 1 calc PR A 1 C14 C -0.1626(10) 0.1017(5) -0.0254(7) 0.082(5) Uani 1 1 d D . . H14A H -0.1999 0.1424 -0.0088 0.124 Uiso 0.534(15) 1 calc PR A 1 H14B H -0.2280 0.0594 -0.0527 0.124 Uiso 0.534(15) 1 calc PR A 1 H14C H -0.1357 0.1296 -0.0539 0.124 Uiso 0.534(15) 1 calc PR A 1 H14D H -0.2412 0.1330 -0.0573 0.124 Uiso 0.466(15) 1 d PR A 2 H14E H -0.0897 0.1401 0.0004 0.124 Uiso 0.466(15) 1 d PR A 2 H14F H -0.1773 0.0708 0.0068 0.124 Uiso 0.466(15) 1 d PR A 2 C15A C -1.0572(18) 0.0687(8) -0.5542(8) 0.058(8) Uani 0.518(19) 1 d PD B 1 H15A H -0.9848 0.1084 -0.5398 0.070 Uiso 0.518(19) 1 calc PR B 1 H15B H -1.1208 0.0975 -0.5466 0.070 Uiso 0.518(19) 1 calc PR B 1 C15B C -1.0710(16) -0.0108(8) -0.5854(7) 0.033(6) Uani 0.482(19) 1 d PD B 2 H15C H -1.0058 -0.0385 -0.5924 0.040 Uiso 0.482(19) 1 calc PR B 2 H15D H -1.1424 -0.0512 -0.5997 0.040 Uiso 0.482(19) 1 calc PR B 2 C16 C -1.1310(11) 0.0624(5) -0.6408(5) 0.051(3) Uani 1 1 d D . . H16A H -1.1549 0.1180 -0.6607 0.077 Uiso 0.518(19) 1 calc PR B 1 H16B H -1.2095 0.0282 -0.6594 0.077 Uiso 0.518(19) 1 calc PR B 1 H16C H -1.0713 0.0372 -0.6524 0.077 Uiso 0.518(19) 1 calc PR B 1 H16D H -1.1664 0.0393 -0.6869 0.077 Uiso 0.482(19) 1 d PR B 2 H16E H -1.0627 0.1026 -0.6310 0.077 Uiso 0.482(19) 1 d PR B 2 H16F H -1.2007 0.0899 -0.6384 0.077 Uiso 0.482(19) 1 d PR B 2 C17A C -0.8786(14) -0.0235(8) -0.5097(11) 0.044(4) Uani 0.520(13) 1 d PD B 1 H17A H -0.8439 -0.0790 -0.4901 0.053 Uiso 0.520(13) 1 calc PR B 1 H17B H -0.9088 -0.0245 -0.5591 0.053 Uiso 0.520(13) 1 calc PR B 1 C17B C -0.8968(15) 0.0601(9) -0.4616(11) 0.044(4) Uani 0.480(13) 1 d PD B 2 H17C H -0.8656 0.0564 -0.4121 0.053 Uiso 0.480(13) 1 calc PR B 2 H17D H -0.9303 0.1168 -0.4776 0.053 Uiso 0.480(13) 1 calc PR B 2 C18 C -0.7748(11) 0.0407(6) -0.4732(7) 0.094(6) Uani 1 1 d D . . H18A H -0.7012 0.0277 -0.4782 0.141 Uiso 0.520(13) 1 calc PR B 1 H18B H -0.7455 0.0411 -0.4243 0.141 Uiso 0.520(13) 1 calc PR B 1 H18C H -0.8098 0.0953 -0.4931 0.141 Uiso 0.520(13) 1 calc PR B 1 H18D H -0.7061 0.0819 -0.4480 0.141 Uiso 0.480(13) 1 d PR B 2 H18E H -0.8059 0.0438 -0.5222 0.141 Uiso 0.480(13) 1 d PR B 2 H18F H -0.7402 -0.0148 -0.4559 0.141 Uiso 0.480(13) 1 d PR B 2 C19 C -0.6148(10) 0.7669(5) -0.0445(6) 0.041(3) Uani 1 1 d . . . H19A H -0.6608 0.7269 -0.0319 0.049 Uiso 1 1 calc R . . H19B H -0.6716 0.8163 -0.0636 0.049 Uiso 1 1 calc R . . C20 C -0.4814(10) 0.7967(6) 0.0286(6) 0.056(3) Uani 1 1 d . . . H20A H -0.4322 0.8360 0.0183 0.084 Uiso 1 1 calc R . . H20B H -0.4271 0.7481 0.0521 0.084 Uiso 1 1 calc R . . H20C H -0.5065 0.8233 0.0583 0.084 Uiso 1 1 calc R . . C21 C -0.7573(9) 0.7038(5) -0.1796(6) 0.044(3) Uani 1 1 d . . . H21A H -0.8025 0.6662 -0.1647 0.053 Uiso 1 1 calc R . . H21B H -0.8067 0.7565 -0.1934 0.053 Uiso 1 1 calc R . . C22 C -0.7730(10) 0.6622(5) -0.2510(6) 0.051(3) Uani 1 1 d . . . H22A H -0.7401 0.7013 -0.2711 0.077 Uiso 1 1 calc R . . H22B H -0.8650 0.6506 -0.2844 0.077 Uiso 1 1 calc R . . H22C H -0.7231 0.6106 -0.2392 0.077 Uiso 1 1 calc R . . C23 C -0.5459(10) 0.7691(4) -0.1444(6) 0.046(3) Uani 1 1 d . . . H23A H -0.4583 0.7896 -0.1092 0.055 Uiso 1 1 calc R . . H23B H -0.5354 0.7287 -0.1737 0.055 Uiso 1 1 calc R . . C24 C -0.6236(12) 0.8372(5) -0.1860(7) 0.077(4) Uani 1 1 d . . . H24A H -0.7099 0.8170 -0.2214 0.115 Uiso 1 1 calc R . . H24B H -0.5814 0.8632 -0.2079 0.115 Uiso 1 1 calc R . . H24C H -0.6325 0.8780 -0.1570 0.115 Uiso 1 1 calc R . . C25 C -0.5134(9) 0.6602(4) -0.0666(6) 0.042(3) Uani 1 1 d . . . H25A H -0.4280 0.6863 -0.0347 0.050 Uiso 1 1 calc R . . H25B H -0.5025 0.6224 -0.0972 0.050 Uiso 1 1 calc R . . C26 C -0.5551(13) 0.6100(5) -0.0249(7) 0.070(4) Uani 1 1 d . . . H26A H -0.5530 0.6454 0.0104 0.106 Uiso 1 1 calc R . . H26B H -0.4955 0.5633 -0.0029 0.106 Uiso 1 1 calc R . . H26C H -0.6437 0.5891 -0.0555 0.106 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0283(4) 0.0084(2) 0.0440(5) -0.0008(3) 0.0225(4) -0.0007(2) S1 0.0357(12) 0.0105(7) 0.0539(16) -0.0016(8) 0.0279(12) -0.0004(7) S2 0.0336(12) 0.0097(7) 0.0676(18) -0.0028(9) 0.0309(12) -0.0020(7) S3 0.0312(12) 0.0128(7) 0.0615(17) 0.0018(8) 0.0301(12) 0.0020(7) S4 0.0343(12) 0.0120(7) 0.0576(17) -0.0004(8) 0.0283(12) 0.0007(7) S5 0.0345(12) 0.0199(8) 0.0482(16) -0.0018(9) 0.0220(12) 0.0014(8) S6 0.0511(15) 0.0192(8) 0.0541(17) 0.0007(9) 0.0360(14) 0.0022(9) N1 0.071(6) 0.014(3) 0.105(8) -0.009(4) 0.059(6) 0.005(3) N2 0.059(6) 0.016(3) 0.104(8) -0.018(4) 0.049(6) -0.015(3) N3 0.069(6) 0.017(3) 0.091(8) 0.015(4) 0.055(6) 0.009(3) N4 0.045(5) 0.014(3) 0.109(9) 0.006(4) 0.036(5) 0.006(3) N5 0.037(4) 0.013(2) 0.064(6) -0.006(3) 0.035(4) -0.004(3) N6 0.034(4) 0.016(3) 0.053(5) -0.002(3) 0.025(4) -0.002(3) N7 0.034(6) 0.007(3) 0.055(8) 0.002(4) 0.023(5) 0.003(3) N8 0.038(4) 0.010(2) 0.056(5) -0.002(3) 0.030(4) 0.000(2) N9 0.058(7) 0.004(3) 0.065(9) 0.000(4) 0.031(7) -0.001(4) C1 0.041(5) 0.014(3) 0.057(7) -0.004(4) 0.028(5) -0.007(3) C2 0.037(5) 0.014(3) 0.047(6) -0.006(3) 0.024(5) 0.000(3) C3 0.036(5) 0.013(2) 0.054(6) -0.005(3) 0.021(5) 0.001(3) C4 0.041(5) 0.013(3) 0.068(7) -0.011(4) 0.031(5) -0.004(3) C5 0.041(5) 0.016(3) 0.055(7) 0.006(4) 0.027(5) 0.007(3) C6 0.025(4) 0.008(2) 0.048(6) -0.002(3) 0.022(4) -0.001(3) C7 0.025(4) 0.007(2) 0.059(7) -0.008(3) 0.016(4) 0.000(3) C8 0.026(5) 0.009(3) 0.078(8) 0.001(4) 0.023(5) -0.001(3) C9 0.026(5) 0.017(3) 0.061(7) -0.001(4) 0.029(5) 0.001(3) C10 0.030(5) 0.013(3) 0.046(6) 0.004(3) 0.022(4) -0.003(3) C11B 0.037(7) 0.003(3) 0.071(9) -0.002(5) 0.037(7) 0.000(4) C11A 0.037(7) 0.003(3) 0.071(9) -0.002(5) 0.037(7) 0.000(4) C12 0.067(7) 0.014(3) 0.167(14) 0.005(5) 0.084(9) -0.006(4) C13A 0.033(10) 0.007(5) 0.084(16) -0.001(7) 0.026(10) -0.001(6) C13B 0.059(14) 0.013(6) 0.041(14) -0.005(7) 0.025(11) -0.007(8) C14 0.055(7) 0.016(4) 0.184(15) -0.007(6) 0.069(9) 0.013(4) C15A 0.052(13) 0.014(6) 0.12(2) 0.033(9) 0.056(14) 0.016(7) C15B 0.030(10) 0.016(6) 0.056(15) -0.014(7) 0.023(10) -0.005(6) C16 0.074(8) 0.029(4) 0.061(8) 0.009(5) 0.044(7) 0.018(5) C17A 0.044(8) 0.009(4) 0.076(11) -0.006(5) 0.030(8) -0.005(5) C17B 0.044(8) 0.009(4) 0.076(11) -0.006(5) 0.030(8) -0.005(5) C18 0.059(8) 0.034(5) 0.136(14) 0.013(7) 0.015(8) -0.030(6) C19 0.053(6) 0.018(3) 0.074(8) -0.018(4) 0.049(6) -0.010(4) C20 0.056(7) 0.035(5) 0.096(10) -0.035(6) 0.052(7) -0.017(5) C21 0.039(6) 0.023(4) 0.071(8) -0.007(4) 0.029(5) -0.005(4) C22 0.049(6) 0.023(4) 0.072(8) -0.012(4) 0.025(6) -0.001(4) C23 0.061(7) 0.013(3) 0.096(9) -0.002(4) 0.063(7) -0.002(4) C24 0.102(10) 0.015(4) 0.162(14) 0.022(6) 0.103(10) 0.014(5) C25 0.041(5) 0.012(3) 0.070(8) 0.004(4) 0.028(5) 0.005(3) C26 0.103(10) 0.020(4) 0.116(12) 0.012(5) 0.077(9) 0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 S2 2.228(2) . ? Mo1 S1 2.264(2) . ? Mo1 S4 2.307(2) . ? Mo1 S3 2.330(2) . ? Mo1 N5 2.384(8) . ? Mo1 N6 2.418(9) . ? S1 C2 1.632(8) . ? S2 C3 1.636(9) . ? S3 C6 1.666(8) . ? S4 C7 1.695(9) . ? S5 C9 1.888(10) . ? S6 C10 1.904(10) . ? N1 C1 1.108(12) . ? N2 C4 1.049(10) . ? N3 C5 1.152(12) . ? N4 C8 1.107(10) . ? N5 C9 1.390(12) . ? N6 C10 1.388(12) . ? N7 C13B 1.494(14) 3 ? N7 C13B 1.494(14) . ? N7 C11B 1.525(12) 3 ? N7 C11B 1.525(12) . ? N7 C13A 1.605(13) . ? N7 C13A 1.605(13) 3 ? N7 C11A 1.615(14) . ? N7 C11A 1.615(14) 3 ? N8 C25 1.435(10) . ? N8 C23 1.519(11) . ? N8 C19 1.620(12) . ? N8 C21 1.682(11) . ? N9 C17B 1.424(13) . ? N9 C17B 1.424(13) 3_354 ? N9 C15A 1.500(12) 3_354 ? N9 C15A 1.500(12) . ? N9 C17A 1.609(14) . ? N9 C17A 1.609(14) 3_354 ? N9 C15B 1.646(13) 3_354 ? N9 C15B 1.646(13) . ? C1 C2 1.365(12) . ? C2 C3 1.356(12) . ? C3 C4 1.343(10) . ? C5 C6 1.404(12) . ? C6 C7 1.384(11) . ? C7 C8 1.395(10) . ? C11B C12 1.639(15) . ? C11B H11A 0.9700 . ? C11B H11B 0.9700 . ? C11B H12E 1.5253 . ? C11B H12F 1.4948 . ? C11A C12 1.567(14) . ? C11A H11C 0.9700 . ? C11A H11D 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C12 H12D 0.9600 . ? C12 H12E 0.9600 . ? C12 H12F 0.9600 . ? C13A C14 1.567(15) . ? C13A H13A 0.9700 . ? C13A H13B 0.9700 . ? C13B C14 1.629(15) . ? C13B H13C 0.9700 . ? C13B H13D 0.9700 . ? C13B H14E 1.5378 . ? C13B H14F 1.4639 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C14 H14D 0.9600 . ? C14 H14E 0.9600 . ? C14 H14F 0.9600 . ? C15A C16 1.660(15) . ? C15A H15A 0.9700 . ? C15A H15B 0.9700 . ? C15B C16 1.567(13) . ? C15B H15C 0.9700 . ? C15B H15D 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C16 H16D 0.9600 . ? C16 H16E 0.9600 . ? C16 H16F 0.9600 . ? C17A C18 1.467(13) . ? C17A H17A 0.9700 . ? C17A H17B 0.9700 . ? C17A H18E 1.4872 . ? C17A H18F 1.4410 . ? C17B C18 1.628(16) . ? C17B H17C 0.9700 . ? C17B H17D 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C18 H18D 0.9600 . ? C18 H18E 0.9600 . ? C18 H18F 0.9600 . ? C19 C20 1.635(14) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C22 1.651(14) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.404(13) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.496(14) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S2 Mo1 S1 87.86(8) . . ? S2 Mo1 S4 69.56(8) . . ? S1 Mo1 S4 130.55(10) . . ? S2 Mo1 S3 120.71(10) . . ? S1 Mo1 S3 69.77(7) . . ? S4 Mo1 S3 84.59(8) . . ? S2 Mo1 N5 140.03(17) . . ? S1 Mo1 N5 88.21(18) . . ? S4 Mo1 N5 136.92(16) . . ? S3 Mo1 N5 94.85(19) . . ? S2 Mo1 N6 90.46(17) . . ? S1 Mo1 N6 135.35(16) . . ? S4 Mo1 N6 89.73(18) . . ? S3 Mo1 N6 143.38(15) . . ? N5 Mo1 N6 65.6(3) . . ? C2 S1 Mo1 103.3(3) . . ? C3 S2 Mo1 103.6(3) . . ? C6 S3 Mo1 107.2(3) . . ? C7 S4 Mo1 105.9(3) . . ? C9 N5 Mo1 165.5(6) . . ? C10 N6 Mo1 167.7(6) . . ? C13B N7 C13B 180.0(13) 3 . ? C13B N7 C11B 107.5(9) 3 3 ? C13B N7 C11B 72.5(9) . 3 ? C13B N7 C11B 72.5(9) 3 . ? C13B N7 C11B 107.5(9) . . ? C11B N7 C11B 180(2) 3 . ? C13B N7 C13A 94.4(8) 3 . ? C13B N7 C13A 85.6(8) . . ? C11B N7 C13A 123.9(7) 3 . ? C11B N7 C13A 56.1(7) . . ? C13B N7 C13A 85.6(8) 3 3 ? C13B N7 C13A 94.4(8) . 3 ? C11B N7 C13A 56.1(7) 3 3 ? C11B N7 C13A 123.9(7) . 3 ? C13A N7 C13A 180.0(19) . 3 ? C13B N7 C11A 123.0(8) 3 . ? C13B N7 C11A 57.0(8) . . ? C11B N7 C11A 95.8(7) 3 . ? C11B N7 C11A 84.2(7) . . ? C13A N7 C11A 114.5(8) . . ? C13A N7 C11A 65.5(8) 3 . ? C13B N7 C11A 57.0(8) 3 3 ? C13B N7 C11A 123.0(8) . 3 ? C11B N7 C11A 84.2(7) 3 3 ? C11B N7 C11A 95.8(7) . 3 ? C13A N7 C11A 65.5(8) . 3 ? C13A N7 C11A 114.5(8) 3 3 ? C11A N7 C11A 180.0(10) . 3 ? C25 N8 C23 104.4(7) . . ? C25 N8 C19 96.0(7) . . ? C23 N8 C19 123.2(6) . . ? C25 N8 C21 123.1(6) . . ? C23 N8 C21 98.4(7) . . ? C19 N8 C21 113.5(6) . . ? C17B N9 C17B 180(3) . 3_354 ? C17B N9 C15A 96.7(10) . 3_354 ? C17B N9 C15A 83.3(10) 3_354 3_354 ? C17B N9 C15A 83.3(10) . . ? C17B N9 C15A 96.7(10) 3_354 . ? C15A N9 C15A 180.000(4) 3_354 . ? C17B N9 C17A 72.1(8) . . ? C17B N9 C17A 107.9(8) 3_354 . ? C15A N9 C17A 83.6(10) 3_354 . ? C15A N9 C17A 96.4(10) . . ? C17B N9 C17A 107.9(8) . 3_354 ? C17B N9 C17A 72.1(8) 3_354 3_354 ? C15A N9 C17A 96.4(10) 3_354 3_354 ? C15A N9 C17A 83.6(10) . 3_354 ? C17A N9 C17A 180.0(14) . 3_354 ? C17B N9 C15B 58.6(10) . 3_354 ? C17B N9 C15B 121.4(10) 3_354 3_354 ? C15A N9 C15B 52.8(8) 3_354 3_354 ? C15A N9 C15B 127.2(8) . 3_354 ? C17A N9 C15B 103.8(9) . 3_354 ? C17A N9 C15B 76.2(9) 3_354 3_354 ? C17B N9 C15B 121.4(10) . . ? C17B N9 C15B 58.6(10) 3_354 . ? C15A N9 C15B 127.2(8) 3_354 . ? C15A N9 C15B 52.8(8) . . ? C17A N9 C15B 76.2(9) . . ? C17A N9 C15B 103.8(9) 3_354 . ? C15B N9 C15B 180.000(4) 3_354 . ? N1 C1 C2 178.4(10) . . ? C3 C2 C1 123.1(8) . . ? C3 C2 S1 122.0(6) . . ? C1 C2 S1 114.9(7) . . ? C4 C3 C2 122.5(8) . . ? C4 C3 S2 114.3(7) . . ? C2 C3 S2 123.2(6) . . ? N2 C4 C3 178.0(10) . . ? N3 C5 C6 177.7(10) . . ? C7 C6 C5 122.8(7) . . ? C7 C6 S3 119.9(7) . . ? C5 C6 S3 117.3(6) . . ? C6 C7 C8 122.1(8) . . ? C6 C7 S4 122.3(6) . . ? C8 C7 S4 115.7(7) . . ? N4 C8 C7 178.5(11) . . ? N5 C9 S5 176.5(7) . . ? N6 C10 S6 177.8(7) . . ? N7 C11B C12 97.2(9) . . ? N7 C11B H11A 112.3 . . ? C12 C11B H11A 112.3 . . ? N7 C11B H11B 112.3 . . ? C12 C11B H11B 112.3 . . ? H11A C11B H11B 109.9 . . ? N7 C11B H12E 109.8 . . ? C12 C11B H12E 35.1 . . ? H11A C11B H12E 77.3 . . ? H11B C11B H12E 129.5 . . ? N7 C11B H12F 111.3 . . ? C12 C11B H12F 35.3 . . ? H11A C11B H12F 128.2 . . ? H11B C11B H12F 77.0 . . ? H12E C11B H12F 62.5 . . ? C12 C11A N7 96.5(9) . . ? C12 C11A H11C 112.5 . . ? N7 C11A H11C 112.5 . . ? C12 C11A H11D 112.5 . . ? N7 C11A H11D 112.5 . . ? H11C C11A H11D 110.0 . . ? C11A C12 C11B 82.1(8) . . ? C11A C12 H12A 168.4 . . ? C11B C12 H12A 109.5 . . ? C11A C12 H12B 64.3 . . ? C11B C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11A C12 H12C 65.9 . . ? C11B C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11A C12 H12D 109.5 . . ? C11B C12 H12D 168.3 . . ? H12A C12 H12D 58.9 . . ? H12B C12 H12D 76.0 . . ? H12C C12 H12D 77.3 . . ? C11A C12 H12E 109.5 . . ? C11B C12 H12E 66.0 . . ? H12A C12 H12E 77.1 . . ? H12B C12 H12E 173.3 . . ? H12C C12 H12E 68.7 . . ? H12D C12 H12E 109.5 . . ? C11A C12 H12F 109.3 . . ? C11B C12 H12F 64.1 . . ? H12A C12 H12F 76.2 . . ? H12B C12 H12F 71.5 . . ? H12C C12 H12F 173.0 . . ? H12D C12 H12F 109.5 . . ? H12E C12 H12F 109.5 . . ? C14 C13A N7 95.0(9) . . ? C14 C13A H13A 112.7 . . ? N7 C13A H13A 112.7 . . ? C14 C13A H13B 112.7 . . ? N7 C13A H13B 112.7 . . ? H13A C13A H13B 110.2 . . ? N7 C13B C14 96.9(9) . . ? N7 C13B H13C 112.4 . . ? C14 C13B H13C 112.4 . . ? N7 C13B H13D 112.4 . . ? C14 C13B H13D 112.4 . . ? H13C C13B H13D 109.9 . . ? N7 C13B H14E 108.4 . . ? C14 C13B H14E 35.1 . . ? H13C C13B H14E 77.4 . . ? H13D C13B H14E 130.8 . . ? N7 C13B H14F 112.3 . . ? C14 C13B H14F 35.7 . . ? H13C C13B H14F 127.2 . . ? H13D C13B H14F 76.7 . . ? H14E C13B H14F 62.9 . . ? C13A C14 C13B 82.5(8) . . ? C13A C14 H14A 167.9 . . ? C13B C14 H14A 109.5 . . ? C13A C14 H14B 62.8 . . ? C13B C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13A C14 H14C 67.1 . . ? C13B C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13A C14 H14D 109.4 . . ? C13B C14 H14D 167.9 . . ? H14A C14 H14D 58.6 . . ? H14B C14 H14D 75.2 . . ? H14C C14 H14D 78.3 . . ? C13A C14 H14E 109.5 . . ? C13B C14 H14E 67.2 . . ? H14A C14 H14E 78.2 . . ? H14B C14 H14E 172.3 . . ? H14C C14 H14E 66.4 . . ? H14D C14 H14E 109.5 . . ? C13A C14 H14F 109.6 . . ? C13B C14 H14F 62.8 . . ? H14A C14 H14F 75.3 . . ? H14B C14 H14F 73.8 . . ? H14C C14 H14F 172.2 . . ? H14D C14 H14F 109.5 . . ? H14E C14 H14F 109.5 . . ? N9 C15A C16 129.7(11) . . ? N9 C15A H15A 104.9 . . ? C16 C15A H15A 104.9 . . ? N9 C15A H15B 104.9 . . ? C16 C15A H15B 104.9 . . ? H15A C15A H15B 105.8 . . ? C16 C15B N9 125.9(9) . . ? C16 C15B H15C 105.9 . . ? N9 C15B H15C 105.9 . . ? C16 C15B H15D 105.9 . . ? N9 C15B H15D 105.9 . . ? H15C C15B H15D 106.2 . . ? C15B C16 C15A 51.6(7) . . ? C15B C16 H16A 161.0 . . ? C15A C16 H16A 109.5 . . ? C15B C16 H16B 81.9 . . ? C15A C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15B C16 H16C 79.5 . . ? C15A C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15B C16 H16D 109.4 . . ? C15A C16 H16D 160.9 . . ? H16A C16 H16D 89.6 . . ? H16B C16 H16D 63.1 . . ? H16C C16 H16D 61.0 . . ? C15B C16 H16E 109.5 . . ? C15A C16 H16E 80.4 . . ? H16A C16 H16E 60.3 . . ? H16B C16 H16E 168.4 . . ? H16C C16 H16E 71.5 . . ? H16D C16 H16E 109.5 . . ? C15B C16 H16F 109.6 . . ? C15A C16 H16F 81.1 . . ? H16A C16 H16F 63.8 . . ? H16B C16 H16F 67.3 . . ? H16C C16 H16F 169.3 . . ? H16D C16 H16F 109.5 . . ? H16E C16 H16F 109.5 . . ? C18 C17A N9 108.1(10) . . ? C18 C17A H17A 110.1 . . ? N9 C17A H17A 110.1 . . ? C18 C17A H17B 110.1 . . ? N9 C17A H17B 110.1 . . ? H17A C17A H17B 108.4 . . ? C18 C17A H18E 37.9 . . ? N9 C17A H18E 120.6 . . ? H17A C17A H18E 125.7 . . ? H17B C17A H18E 72.2 . . ? C18 C17A H18F 38.5 . . ? N9 C17A H18F 124.7 . . ? H17A C17A H18F 71.6 . . ? H17B C17A H18F 121.9 . . ? H18E C17A H18F 64.7 . . ? N9 C17B C18 109.2(11) . . ? N9 C17B H17C 109.8 . . ? C18 C17B H17C 109.8 . . ? N9 C17B H17D 109.8 . . ? C18 C17B H17D 109.8 . . ? H17C C17B H17D 108.3 . . ? C17A C18 C17B 70.5(9) . . ? C17A C18 H18A 109.5 . . ? C17B C18 H18A 177.5 . . ? C17A C18 H18B 109.5 . . ? C17B C18 H18B 68.4 . . ? H18A C18 H18B 109.5 . . ? C17A C18 H18C 109.5 . . ? C17B C18 H18C 72.7 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17A C18 H18D 178.3 . . ? C17B C18 H18D 109.1 . . ? H18A C18 H18D 70.9 . . ? H18B C18 H18D 68.9 . . ? H18C C18 H18D 71.8 . . ? C17A C18 H18E 72.2 . . ? C17B C18 H18E 109.8 . . ? H18A C18 H18E 72.4 . . ? H18B C18 H18E 176.5 . . ? H18C C18 H18E 67.1 . . ? H18D C18 H18E 109.5 . . ? C17A C18 H18F 69.3 . . ? C17B C18 H18F 109.5 . . ? H18A C18 H18F 68.4 . . ? H18B C18 H18F 74.0 . . ? H18C C18 H18F 176.5 . . ? H18D C18 H18F 109.5 . . ? H18E C18 H18F 109.5 . . ? N8 C19 C20 121.9(7) . . ? N8 C19 H19A 106.8 . . ? C20 C19 H19A 106.8 . . ? N8 C19 H19B 106.8 . . ? C20 C19 H19B 106.8 . . ? H19A C19 H19B 106.7 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 N8 121.6(7) . . ? C22 C21 H21A 106.9 . . ? N8 C21 H21A 106.9 . . ? C22 C21 H21B 106.9 . . ? N8 C21 H21B 106.9 . . ? H21A C21 H21B 106.7 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 N8 112.2(8) . . ? C24 C23 H23A 109.2 . . ? N8 C23 H23A 109.2 . . ? C24 C23 H23B 109.2 . . ? N8 C23 H23B 109.2 . . ? H23A C23 H23B 107.9 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N8 C25 C26 112.7(8) . . ? N8 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? N8 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.28 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.871 _refine_diff_density_min -0.744 _refine_diff_density_rms 0.176 _ccdc_chemical_compound_source_recrystallisation Dichloromethane #===END # Attachment 'CIFs_Sarkar.cif' data_13apram _database_code_depnum_ccdc_archive 'CCDC 691999' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C33 H22 Mo N4 P S5 , C8 H20 N, C H2 Cl2' _chemical_formula_sum 'C42 H44 Cl2 Mo N5 P S5' _chemical_formula_weight 976.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.086(5) _cell_length_b 11.646(5) _cell_length_c 18.305(5) _cell_angle_alpha 100.126(5) _cell_angle_beta 101.684(5) _cell_angle_gamma 97.983(5) _cell_volume 2240.7(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.30 _exptl_crystal_description Needle _exptl_crystal_colour Violet _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 988 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9442 _exptl_absorpt_correction_T_max 0.9722 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71069 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14920 _diffrn_reflns_av_R_equivalents 0.0404 _diffrn_reflns_av_sigmaI/netI 0.0975 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 28.30 _reflns_number_total 10640 _reflns_number_gt 7697 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628(Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45(Bruker, 2003)' _computing_data_reduction 'SAINT 6.45(Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e, ORTEP' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+23.5508P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10640 _refine_ls_number_parameters 533 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1154 _refine_ls_R_factor_gt 0.0751 _refine_ls_wR_factor_ref 0.2109 _refine_ls_wR_factor_gt 0.1509 _refine_ls_goodness_of_fit_ref 1.147 _refine_ls_restrained_S_all 1.152 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.71656(5) 0.21664(5) 0.77094(3) 0.01555(14) Uani 1 1 d . . . P1 P 0.60523(16) 0.11957(15) 0.86197(10) 0.0184(4) Uani 1 1 d . . . S1 S 0.50914(15) 0.23779(16) 0.72062(10) 0.0210(4) Uani 1 1 d . . . S2 S 0.72107(17) 0.17865(18) 0.63950(10) 0.0273(4) Uani 1 1 d . . . S3 S 0.72327(15) 0.37837(14) 0.86943(9) 0.0184(3) Uani 1 1 d . . . S4 S 0.92259(17) 0.31457(16) 0.78092(11) 0.0251(4) Uani 1 1 d . . . S5 S 0.80497(16) 0.04159(14) 0.77629(10) 0.0209(4) Uani 1 1 d . . . Cl1 Cl 1.1810(3) 0.3949(3) 0.6921(2) 0.0981(14) Uani 1 1 d . . . Cl2 Cl 0.9987(3) 0.3744(3) 0.5482(3) 0.0904(12) Uani 1 1 d . . . N1 N 0.2764(7) 0.2374(7) 0.5386(4) 0.0433(19) Uani 1 1 d . . . N2 N 0.5323(8) 0.1588(10) 0.4409(4) 0.067(3) Uani 1 1 d . . . N3 N 0.9095(6) 0.6509(6) 1.0023(4) 0.0295(14) Uani 1 1 d . . . N4 N 1.1687(6) 0.5821(6) 0.8718(4) 0.0357(16) Uani 1 1 d . . . N5 N 0.7228(7) 0.6142(5) 0.6781(4) 0.0304(15) Uani 1 1 d . . . C1 C 0.4840(6) 0.2138(6) 0.6223(4) 0.0214(14) Uani 1 1 d . . . C2 C 0.3664(7) 0.2268(6) 0.5772(4) 0.0248(15) Uani 1 1 d . . . C3 C 0.5768(7) 0.1892(6) 0.5872(4) 0.0228(14) Uani 1 1 d . . . C4 C 0.5548(8) 0.1717(9) 0.5057(5) 0.040(2) Uani 1 1 d . . . C5 C 0.9547(7) 0.4430(6) 0.8508(4) 0.0232(15) Uani 1 1 d . . . C6 C 1.0734(7) 0.5191(6) 0.8631(4) 0.0268(16) Uani 1 1 d . . . C7 C 0.8713(6) 0.4694(5) 0.8913(4) 0.0186(13) Uani 1 1 d . . . C8 C 0.8937(7) 0.5709(6) 0.9528(4) 0.0222(14) Uani 1 1 d . . . C9 C 0.9168(6) 0.0259(6) 0.7180(4) 0.0218(14) Uani 1 1 d . . . C10 C 0.8776(7) -0.0349(6) 0.6408(4) 0.0241(15) Uani 1 1 d . . . H10 H 0.7928 -0.0598 0.6181 0.029 Uiso 1 1 calc R . . C11 C 0.9653(7) -0.0567(7) 0.5997(4) 0.0294(17) Uani 1 1 d . . . H11 H 0.9383 -0.0954 0.5487 0.035 Uiso 1 1 calc R . . C12 C 1.0938(7) -0.0230(6) 0.6316(4) 0.0268(16) Uani 1 1 d . . . C13 C 1.1309(7) 0.0372(7) 0.7074(5) 0.0290(17) Uani 1 1 d . . . H13 H 1.2158 0.0619 0.7300 0.035 Uiso 1 1 calc R . . C14 C 1.0439(7) 0.0613(6) 0.7500(4) 0.0257(15) Uani 1 1 d . . . H14 H 1.0712 0.1016 0.8006 0.031 Uiso 1 1 calc R . . C15 C 1.1884(8) -0.0530(8) 0.5859(5) 0.0370(19) Uani 1 1 d . . . H15A H 1.1455 -0.0944 0.5351 0.055 Uiso 1 1 calc R . . H15B H 1.2393 -0.1025 0.6098 0.055 Uiso 1 1 calc R . . H15C H 1.2406 0.0187 0.5836 0.055 Uiso 1 1 calc R . . C16 C 0.7149(7) 0.0714(5) 0.9345(4) 0.0176(13) Uani 1 1 d . . . C17 C 0.6955(7) -0.0381(6) 0.9518(4) 0.0233(15) Uani 1 1 d . . . H17 H 0.6236 -0.0925 0.9254 0.028 Uiso 1 1 calc R . . C18 C 0.7813(8) -0.0701(7) 1.0083(5) 0.0324(18) Uani 1 1 d . . . H18 H 0.7659 -0.1451 1.0192 0.039 Uiso 1 1 calc R . . C19 C 0.8875(7) 0.0078(7) 1.0474(4) 0.0296(17) Uani 1 1 d . . . H19 H 0.9450 -0.0139 1.0846 0.036 Uiso 1 1 calc R . . C20 C 0.9090(7) 0.1198(7) 1.0314(4) 0.0272(16) Uani 1 1 d . . . H20 H 0.9796 0.1746 1.0594 0.033 Uiso 1 1 calc R . . C21 C 0.8237(6) 0.1511(6) 0.9725(4) 0.0212(14) Uani 1 1 d . . . H21 H 0.8405 0.2244 0.9594 0.025 Uiso 1 1 calc R . . C22 C 0.4846(7) -0.0113(6) 0.8187(4) 0.0223(14) Uani 1 1 d . . . C23 C 0.4024(6) -0.0518(6) 0.8621(4) 0.0211(14) Uani 1 1 d . . . H23 H 0.4075 -0.0091 0.9109 0.025 Uiso 1 1 calc R . . C24 C 0.3155(7) -0.1527(6) 0.8329(4) 0.0264(16) Uani 1 1 d . . . H24 H 0.2625 -0.1787 0.8623 0.032 Uiso 1 1 calc R . . C25 C 0.3048(7) -0.2177(6) 0.7598(4) 0.0282(16) Uani 1 1 d . . . H25 H 0.2460 -0.2873 0.7406 0.034 Uiso 1 1 calc R . . C26 C 0.3824(7) -0.1775(6) 0.7162(4) 0.0258(15) Uani 1 1 d . . . H26 H 0.3739 -0.2195 0.6668 0.031 Uiso 1 1 calc R . . C27 C 0.4745(6) -0.0743(6) 0.7446(4) 0.0188(13) Uani 1 1 d . . . H27 H 0.5272 -0.0486 0.7149 0.023 Uiso 1 1 calc R . . C28 C 0.5232(6) 0.2158(6) 0.9169(4) 0.0192(13) Uani 1 1 d . . . C29 C 0.4106(7) 0.2428(6) 0.8800(4) 0.0243(15) Uani 1 1 d . . . H29 H 0.3753 0.2081 0.8290 0.029 Uiso 1 1 calc R . . C30 C 0.3523(7) 0.3212(7) 0.9196(5) 0.0281(16) Uani 1 1 d . . . H30 H 0.2780 0.3396 0.8947 0.034 Uiso 1 1 calc R . . C31 C 0.4018(7) 0.3727(7) 0.9953(5) 0.0296(17) Uani 1 1 d . . . H31 H 0.3619 0.4266 1.0207 0.035 Uiso 1 1 calc R . . C32 C 0.5106(7) 0.3446(6) 1.0333(4) 0.0258(16) Uani 1 1 d . . . H32 H 0.5431 0.3773 1.0849 0.031 Uiso 1 1 calc R . . C33 C 0.5717(7) 0.2666(6) 0.9937(4) 0.0264(16) Uani 1 1 d . . . H33 H 0.6459 0.2484 1.0191 0.032 Uiso 1 1 calc R . . C34 C 1.0618(10) 0.3009(10) 0.6195(6) 0.057(3) Uani 1 1 d . . . H34A H 0.9954 0.2694 0.6417 0.069 Uiso 1 1 calc R . . H34B H 1.0953 0.2347 0.5963 0.069 Uiso 1 1 calc R . . C35A C 0.8580(14) 0.5706(11) 0.6896(9) 0.031(3) Uani 0.532(12) 1 d P A 1 H35A H 0.8770 0.5425 0.7367 0.038 Uiso 0.532(12) 1 calc PR A 1 H35B H 0.8586 0.5077 0.6473 0.038 Uiso 0.532(12) 1 calc PR A 1 C35B C 0.8125(14) 0.7138(13) 0.6725(11) 0.031(3) Uani 0.468(12) 1 d PD A 2 H35C H 0.8076 0.7845 0.7080 0.038 Uiso 0.468(12) 1 calc PR A 2 H35D H 0.7936 0.7288 0.6213 0.038 Uiso 0.468(12) 1 calc PR A 2 C36 C 0.9525(11) 0.6827(15) 0.6923(11) 0.149(10) Uani 1 1 d D . . H36A H 1.0353 0.6644 0.6990 0.224 Uiso 0.532(12) 1 calc PR A 1 H36B H 0.9496 0.7440 0.7342 0.224 Uiso 0.532(12) 1 calc PR A 1 H36C H 0.9313 0.7094 0.6454 0.224 Uiso 0.532(12) 1 calc PR A 1 H36D H 1.0127 0.7482 0.6890 0.224 Uiso 0.468(12) 1 d PR A 2 H36E H 0.9556 0.6137 0.6559 0.224 Uiso 0.468(12) 1 d PR A 2 H36F H 0.9715 0.6670 0.7428 0.224 Uiso 0.468(12) 1 d PR A 2 C37A C 0.6950(16) 0.6298(11) 0.5957(9) 0.035(3) Uani 0.520(13) 1 d PD A 1 H37A H 0.7593 0.6891 0.5881 0.043 Uiso 0.520(13) 1 calc PR A 1 H37B H 0.6145 0.6539 0.5824 0.043 Uiso 0.520(13) 1 calc PR A 1 C37B C 0.7262(17) 0.4949(13) 0.6355(9) 0.035(3) Uani 0.480(13) 1 d PD A 2 H37C H 0.6647 0.4356 0.6456 0.043 Uiso 0.480(13) 1 calc PR A 2 H37D H 0.8084 0.4747 0.6502 0.043 Uiso 0.480(13) 1 calc PR A 2 C38 C 0.6938(14) 0.5008(12) 0.5448(7) 0.110(6) Uani 1 1 d D . . H38A H 0.6762 0.5041 0.4918 0.166 Uiso 0.520(13) 1 calc PR A 1 H38B H 0.6304 0.4433 0.5536 0.166 Uiso 0.520(13) 1 calc PR A 1 H38C H 0.7741 0.4785 0.5589 0.166 Uiso 0.520(13) 1 calc PR A 1 H38D H 0.6947 0.4247 0.5147 0.166 Uiso 0.480(13) 1 d PR A 2 H38E H 0.7555 0.5596 0.5357 0.166 Uiso 0.480(13) 1 d PR A 2 H38F H 0.6125 0.5211 0.5310 0.166 Uiso 0.480(13) 1 d PR A 2 C39A C 0.7420(14) 0.7322(11) 0.7296(8) 0.026(4) Uani 0.527(18) 1 d P A 1 H39A H 0.6759 0.7735 0.7107 0.031 Uiso 0.527(18) 1 calc PR A 1 H39B H 0.8210 0.7782 0.7279 0.031 Uiso 0.527(18) 1 calc PR A 1 C39B C 0.7208(18) 0.6071(12) 0.7628(10) 0.035(5) Uani 0.473(18) 1 d P A 2 H39C H 0.6402 0.5633 0.7637 0.041 Uiso 0.473(18) 1 calc PR A 2 H39D H 0.7846 0.5637 0.7819 0.041 Uiso 0.473(18) 1 calc PR A 2 C40 C 0.743(2) 0.7263(11) 0.8145(6) 0.137(9) Uani 1 1 d . . . H40A H 0.7556 0.8053 0.8445 0.205 Uiso 0.527(18) 1 calc PR A 1 H40B H 0.8094 0.6874 0.8342 0.205 Uiso 0.527(18) 1 calc PR A 1 H40C H 0.6642 0.6826 0.8169 0.205 Uiso 0.527(18) 1 calc PR A 1 H40D H 0.7405 0.7169 0.8653 0.205 Uiso 0.473(18) 1 d PR A 2 H40E H 0.6791 0.7694 0.7966 0.205 Uiso 0.473(18) 1 d PR A 2 H40F H 0.8235 0.7692 0.8148 0.205 Uiso 0.473(18) 1 d PR A 2 C41A C 0.6379(14) 0.5182(13) 0.6924(9) 0.035(4) Uani 0.523(18) 1 d PD A 1 H41A H 0.6601 0.5125 0.7455 0.042 Uiso 0.523(18) 1 calc PR A 1 H41B H 0.6416 0.4432 0.6608 0.042 Uiso 0.523(18) 1 calc PR A 1 C41B C 0.5868(15) 0.6441(13) 0.6443(10) 0.032(5) Uani 0.477(18) 1 d P A 2 H41C H 0.5808 0.7248 0.6659 0.039 Uiso 0.477(18) 1 calc PR A 2 H41D H 0.5689 0.6325 0.5891 0.039 Uiso 0.477(18) 1 calc PR A 2 C42 C 0.4963(11) 0.5505(9) 0.6709(11) 0.121(8) Uani 1 1 d D . . H42A H 0.4364 0.4891 0.6792 0.181 Uiso 0.523(18) 1 calc PR A 1 H42B H 0.4759 0.5564 0.6184 0.181 Uiso 0.523(18) 1 calc PR A 1 H42C H 0.4941 0.6247 0.7028 0.181 Uiso 0.523(18) 1 calc PR A 1 H42D H 0.4124 0.5625 0.6528 0.181 Uiso 0.477(18) 1 d PR A 2 H42E H 0.5147 0.5613 0.7255 0.181 Uiso 0.477(18) 1 d PR A 2 H42F H 0.5038 0.4714 0.6489 0.181 Uiso 0.477(18) 1 d PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0165(3) 0.0133(3) 0.0172(3) 0.0032(2) 0.0044(2) 0.00318(19) P1 0.0202(9) 0.0160(8) 0.0196(9) 0.0024(7) 0.0074(7) 0.0025(6) S1 0.0146(8) 0.0277(9) 0.0201(8) 0.0022(7) 0.0040(6) 0.0056(6) S2 0.0232(9) 0.0454(11) 0.0190(9) 0.0097(8) 0.0097(7) 0.0149(8) S3 0.0187(8) 0.0179(8) 0.0187(8) 0.0039(6) 0.0038(6) 0.0046(6) S4 0.0234(9) 0.0210(8) 0.0315(10) 0.0021(7) 0.0121(7) 0.0018(7) S5 0.0226(9) 0.0157(7) 0.0256(9) 0.0036(7) 0.0070(7) 0.0062(6) Cl1 0.072(2) 0.109(3) 0.084(2) -0.047(2) 0.0507(19) -0.0419(19) Cl2 0.083(2) 0.077(2) 0.138(3) 0.043(2) 0.052(2) 0.0393(19) N1 0.035(4) 0.056(5) 0.031(4) -0.009(3) -0.001(3) 0.018(4) N2 0.040(5) 0.143(10) 0.023(4) 0.021(5) 0.011(3) 0.031(5) N3 0.026(3) 0.031(3) 0.030(4) 0.002(3) 0.004(3) 0.010(3) N4 0.026(3) 0.026(3) 0.049(4) -0.001(3) 0.010(3) -0.009(3) N5 0.048(4) 0.019(3) 0.020(3) 0.005(3) -0.002(3) 0.004(3) C1 0.019(3) 0.019(3) 0.027(4) 0.002(3) 0.008(3) 0.003(3) C2 0.019(3) 0.029(4) 0.023(4) -0.004(3) 0.001(3) 0.011(3) C3 0.029(4) 0.024(3) 0.021(3) 0.007(3) 0.013(3) 0.010(3) C4 0.030(4) 0.073(7) 0.025(4) 0.014(4) 0.012(3) 0.020(4) C5 0.026(4) 0.022(3) 0.027(4) 0.011(3) 0.006(3) 0.013(3) C6 0.029(4) 0.023(4) 0.032(4) 0.006(3) 0.014(3) 0.007(3) C7 0.024(3) 0.008(3) 0.022(3) 0.004(2) -0.001(3) 0.005(2) C8 0.022(4) 0.029(4) 0.016(3) 0.007(3) 0.001(3) 0.008(3) C9 0.017(3) 0.025(3) 0.025(4) 0.011(3) 0.004(3) 0.000(3) C10 0.024(4) 0.020(3) 0.026(4) -0.003(3) 0.008(3) 0.001(3) C11 0.032(4) 0.026(4) 0.026(4) -0.004(3) 0.003(3) 0.005(3) C12 0.028(4) 0.020(3) 0.031(4) 0.001(3) 0.007(3) 0.005(3) C13 0.016(3) 0.028(4) 0.039(4) 0.008(3) 0.000(3) -0.003(3) C14 0.025(4) 0.024(4) 0.025(4) 0.002(3) 0.002(3) 0.002(3) C15 0.033(4) 0.041(5) 0.042(5) 0.008(4) 0.015(4) 0.013(4) C16 0.034(4) 0.011(3) 0.013(3) 0.008(2) 0.013(3) 0.002(3) C17 0.026(4) 0.027(4) 0.022(4) 0.008(3) 0.014(3) 0.006(3) C18 0.043(5) 0.025(4) 0.040(5) 0.018(4) 0.018(4) 0.017(3) C19 0.031(4) 0.039(4) 0.029(4) 0.020(4) 0.013(3) 0.016(3) C20 0.028(4) 0.034(4) 0.021(4) 0.012(3) 0.003(3) 0.007(3) C21 0.023(4) 0.025(3) 0.023(3) 0.016(3) 0.009(3) 0.012(3) C22 0.023(4) 0.021(3) 0.026(4) 0.003(3) 0.012(3) 0.008(3) C23 0.026(4) 0.021(3) 0.023(4) 0.007(3) 0.018(3) 0.004(3) C24 0.027(4) 0.024(4) 0.031(4) 0.008(3) 0.012(3) 0.005(3) C25 0.031(4) 0.022(4) 0.030(4) 0.004(3) 0.008(3) 0.001(3) C26 0.029(4) 0.020(3) 0.026(4) 0.005(3) 0.003(3) -0.001(3) C27 0.014(3) 0.022(3) 0.023(3) 0.007(3) 0.007(3) 0.003(2) C28 0.017(3) 0.014(3) 0.024(4) 0.003(3) 0.001(3) 0.004(2) C29 0.022(4) 0.022(3) 0.031(4) 0.010(3) 0.008(3) 0.004(3) C30 0.027(4) 0.029(4) 0.040(5) 0.016(3) 0.020(3) 0.013(3) C31 0.033(4) 0.027(4) 0.035(4) 0.005(3) 0.020(3) 0.008(3) C32 0.031(4) 0.025(4) 0.019(3) -0.007(3) 0.010(3) 0.005(3) C33 0.034(4) 0.020(3) 0.025(4) -0.004(3) 0.012(3) 0.006(3) C34 0.061(7) 0.059(6) 0.053(6) -0.002(5) 0.039(5) -0.002(5) C35A 0.033(6) 0.009(4) 0.046(7) 0.004(4) -0.001(5) 0.002(4) C35B 0.033(6) 0.009(4) 0.046(7) 0.004(4) -0.001(5) 0.002(4) C36 0.052(8) 0.171(17) 0.21(2) 0.144(16) -0.048(10) -0.051(9) C37A 0.044(7) 0.013(5) 0.043(7) 0.005(5) 0.003(5) -0.001(4) C37B 0.044(7) 0.013(5) 0.043(7) 0.005(5) 0.003(5) -0.001(4) C38 0.100(11) 0.119(13) 0.072(9) -0.058(9) 0.037(8) -0.043(9) C39A 0.031(8) 0.014(6) 0.030(8) 0.005(5) 0.001(6) 0.003(5) C39B 0.048(11) 0.005(6) 0.046(11) 0.010(7) -0.002(8) 0.001(6) C40 0.34(3) 0.052(7) 0.016(5) 0.010(5) 0.016(9) 0.074(12) C41A 0.056(11) 0.024(8) 0.031(8) 0.016(6) 0.010(7) 0.015(7) C41B 0.035(10) 0.017(7) 0.034(9) -0.010(7) -0.007(7) 0.010(6) C42 0.087(10) 0.023(5) 0.26(2) -0.016(8) 0.123(13) -0.013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 S3 2.3487(19) . ? Mo1 S1 2.361(2) . ? Mo1 S4 2.363(2) . ? Mo1 S2 2.381(2) . ? Mo1 S5 2.3900(19) . ? Mo1 P1 2.5857(19) . ? P1 C22 1.822(7) . ? P1 C28 1.831(7) . ? P1 C16 1.831(7) . ? S1 C1 1.731(7) . ? S2 C3 1.722(7) . ? S3 C7 1.755(7) . ? S4 C5 1.731(8) . ? S5 C9 1.799(7) . ? Cl1 C34 1.757(11) . ? Cl2 C34 1.764(12) . ? N1 C2 1.135(9) . ? N2 C4 1.140(11) . ? N3 C8 1.146(9) . ? N4 C6 1.164(9) . ? N5 C35B 1.452(16) . ? N5 C41A 1.454(16) . ? N5 C37B 1.479(17) . ? N5 C39A 1.484(14) . ? N5 C37A 1.526(17) . ? N5 C39B 1.572(19) . ? N5 C41B 1.619(17) . ? N5 C35A 1.633(16) . ? C1 C3 1.355(9) . ? C1 C2 1.437(9) . ? C3 C4 1.435(10) . ? C5 C7 1.332(10) . ? C5 C6 1.433(10) . ? C7 C8 1.437(9) . ? C9 C14 1.385(10) . ? C9 C10 1.415(10) . ? C10 C11 1.369(10) . ? C10 H10 0.9300 . ? C11 C12 1.398(10) . ? C11 H11 0.9300 . ? C12 C13 1.390(11) . ? C12 C15 1.509(11) . ? C13 C14 1.385(11) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.366(9) . ? C16 C21 1.386(10) . ? C17 C18 1.396(10) . ? C17 H17 0.9300 . ? C18 C19 1.362(12) . ? C18 H18 0.9300 . ? C19 C20 1.386(10) . ? C19 H19 0.9300 . ? C20 C21 1.419(9) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C27 1.397(9) . ? C22 C23 1.411(9) . ? C23 C24 1.361(10) . ? C23 H23 0.9300 . ? C24 C25 1.389(10) . ? C24 H24 0.9300 . ? C25 C26 1.377(10) . ? C25 H25 0.9300 . ? C26 C27 1.408(9) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C33 1.389(10) . ? C28 C29 1.398(9) . ? C29 C30 1.378(10) . ? C29 H29 0.9300 . ? C30 C31 1.373(11) . ? C30 H30 0.9300 . ? C31 C32 1.378(11) . ? C31 H31 0.9300 . ? C32 C33 1.396(9) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35A C36 1.543(18) . ? C35A H35A 0.9700 . ? C35A H35B 0.9700 . ? C35A H36E 1.4260 . ? C35A H36F 1.5873 . ? C35B C36 1.626(15) . ? C35B H35C 0.9700 . ? C35B H35D 0.9700 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C36 H36D 0.9600 . ? C36 H36E 0.9600 . ? C36 H36F 0.9600 . ? C37A C38 1.619(14) . ? C37A H37A 0.9700 . ? C37A H37B 0.9700 . ? C37A H38E 1.5689 . ? C37B C38 1.641(15) . ? C37B H37C 0.9700 . ? C37B H37D 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C38 H38D 0.9600 . ? C38 H38E 0.9600 . ? C38 H38F 0.9600 . ? C39A C40 1.567(18) . ? C39A H39A 0.9700 . ? C39A H39B 0.9700 . ? C39A H40E 1.5564 . ? C39A H40F 1.5885 . ? C39B C40 1.494(18) . ? C39B H39C 0.9700 . ? C39B H39D 0.9700 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C40 H40D 0.9600 . ? C40 H40E 0.9600 . ? C40 H40F 0.9600 . ? C41A C42 1.651(15) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C41A H42F 1.5113 . ? C41B C42 1.59(2) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C42 H42D 0.9600 . ? C42 H42E 0.9600 . ? C42 H42F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S3 Mo1 S1 86.78(6) . . ? S3 Mo1 S4 81.93(7) . . ? S1 Mo1 S4 138.28(7) . . ? S3 Mo1 S2 139.01(7) . . ? S1 Mo1 S2 82.12(6) . . ? S4 Mo1 S2 80.69(7) . . ? S3 Mo1 S5 129.51(7) . . ? S1 Mo1 S5 130.12(7) . . ? S4 Mo1 S5 86.07(7) . . ? S2 Mo1 S5 85.85(7) . . ? S3 Mo1 P1 77.16(6) . . ? S1 Mo1 P1 80.61(7) . . ? S4 Mo1 P1 134.36(7) . . ? S2 Mo1 P1 138.43(7) . . ? S5 Mo1 P1 77.17(6) . . ? C22 P1 C28 102.5(3) . . ? C22 P1 C16 104.5(3) . . ? C28 P1 C16 104.2(3) . . ? C22 P1 Mo1 116.8(2) . . ? C28 P1 Mo1 115.1(2) . . ? C16 P1 Mo1 112.2(2) . . ? C1 S1 Mo1 108.4(2) . . ? C3 S2 Mo1 108.2(2) . . ? C7 S3 Mo1 108.8(2) . . ? C5 S4 Mo1 108.7(3) . . ? C9 S5 Mo1 112.8(2) . . ? C35B N5 C41A 174.0(11) . . ? C35B N5 C37B 118.3(11) . . ? C41A N5 C37B 65.3(9) . . ? C35B N5 C39A 58.3(9) . . ? C41A N5 C39A 117.2(10) . . ? C37B N5 C39A 169.5(10) . . ? C35B N5 C37A 71.8(9) . . ? C41A N5 C37A 114.1(9) . . ? C37B N5 C37A 77.9(8) . . ? C39A N5 C37A 108.7(8) . . ? C35B N5 C39B 113.1(10) . . ? C41A N5 C39B 61.0(9) . . ? C37B N5 C39B 108.8(9) . . ? C39A N5 C39B 66.6(8) . . ? C37A N5 C39B 166.5(11) . . ? C35B N5 C41B 105.0(9) . . ? C41A N5 C41B 77.7(9) . . ? C37B N5 C41B 106.7(9) . . ? C39A N5 C41B 83.8(8) . . ? C37A N5 C41B 62.8(9) . . ? C39B N5 C41B 103.7(10) . . ? C35B N5 C35A 74.2(8) . . ? C41A N5 C35A 104.5(8) . . ? C37B N5 C35A 62.8(9) . . ? C39A N5 C35A 107.1(8) . . ? C37A N5 C35A 104.0(10) . . ? C39B N5 C35A 89.5(9) . . ? C41B N5 C35A 165.5(10) . . ? C3 C1 C2 119.2(7) . . ? C3 C1 S1 120.6(6) . . ? C2 C1 S1 120.1(5) . . ? N1 C2 C1 176.5(9) . . ? C1 C3 C4 119.8(7) . . ? C1 C3 S2 120.7(6) . . ? C4 C3 S2 119.6(5) . . ? N2 C4 C3 177.0(9) . . ? C7 C5 C6 121.7(7) . . ? C7 C5 S4 120.7(6) . . ? C6 C5 S4 117.6(5) . . ? N4 C6 C5 178.5(9) . . ? C5 C7 C8 123.9(7) . . ? C5 C7 S3 119.7(5) . . ? C8 C7 S3 116.3(5) . . ? N3 C8 C7 178.7(8) . . ? C14 C9 C10 118.6(7) . . ? C14 C9 S5 120.5(6) . . ? C10 C9 S5 120.5(5) . . ? C11 C10 C9 119.7(7) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 122.3(7) . . ? C10 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C13 C12 C11 117.4(7) . . ? C13 C12 C15 121.5(7) . . ? C11 C12 C15 121.2(7) . . ? C14 C13 C12 121.4(7) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C9 C14 C13 120.7(7) . . ? C9 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 119.3(6) . . ? C17 C16 P1 123.5(6) . . ? C21 C16 P1 117.2(5) . . ? C16 C17 C18 121.3(7) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C19 C18 C17 120.3(7) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 119.5(7) . . ? C18 C19 H19 120.2 . . ? C20 C19 H19 120.2 . . ? C19 C20 C21 120.1(7) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C16 C21 C20 119.3(6) . . ? C16 C21 H21 120.3 . . ? C20 C21 H21 120.3 . . ? C27 C22 C23 119.5(6) . . ? C27 C22 P1 121.5(5) . . ? C23 C22 P1 118.9(5) . . ? C24 C23 C22 120.4(7) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 121.1(7) . . ? C23 C24 H24 119.4 . . ? C25 C24 H24 119.4 . . ? C26 C25 C24 119.0(7) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C25 C26 C27 121.6(7) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C22 C27 C26 118.3(6) . . ? C22 C27 H27 120.8 . . ? C26 C27 H27 120.8 . . ? C33 C28 C29 118.7(7) . . ? C33 C28 P1 122.0(5) . . ? C29 C28 P1 119.2(5) . . ? C30 C29 C28 119.7(7) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C31 C30 C29 121.3(7) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C30 C31 C32 120.0(7) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C33 119.4(7) . . ? C31 C32 H32 120.3 . . ? C33 C32 H32 120.3 . . ? C28 C33 C32 120.9(7) . . ? C28 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? Cl1 C34 Cl2 112.5(6) . . ? Cl1 C34 H34A 109.1 . . ? Cl2 C34 H34A 109.1 . . ? Cl1 C34 H34B 109.1 . . ? Cl2 C34 H34B 109.1 . . ? H34A C34 H34B 107.8 . . ? C36 C35A N5 104.2(10) . . ? C36 C35A H35A 110.9 . . ? N5 C35A H35A 110.9 . . ? C36 C35A H35B 110.9 . . ? N5 C35A H35B 110.9 . . ? H35A C35A H35B 108.9 . . ? C36 C35A H36E 37.5 . . ? N5 C35A H36E 123.2 . . ? H35A C35A H36E 120.8 . . ? H35B C35A H36E 73.7 . . ? C36 C35A H36F 35.7 . . ? N5 C35A H36F 114.4 . . ? H35A C35A H36F 75.5 . . ? H35B C35A H36F 128.9 . . ? H36E C35A H36F 62.4 . . ? N5 C35B C36 108.9(10) . . ? N5 C35B H35C 109.9 . . ? C36 C35B H35C 109.9 . . ? N5 C35B H35D 109.9 . . ? C36 C35B H35D 109.9 . . ? H35C C35B H35D 108.3 . . ? C35A C36 C35B 72.1(9) . . ? C35A C36 H36A 109.5 . . ? C35B C36 H36A 174.5 . . ? C35A C36 H36B 109.5 . . ? C35B C36 H36B 74.4 . . ? H36A C36 H36B 109.5 . . ? C35A C36 H36C 109.5 . . ? C35B C36 H36C 65.2 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35A C36 H36D 174.0 . . ? C35B C36 H36D 109.6 . . ? H36A C36 H36D 68.2 . . ? H36B C36 H36D 76.5 . . ? H36C C36 H36D 67.0 . . ? C35A C36 H36E 64.6 . . ? C35B C36 H36E 108.4 . . ? H36A C36 H36E 68.3 . . ? H36B C36 H36E 171.3 . . ? H36C C36 H36E 79.0 . . ? H36D C36 H36E 109.5 . . ? C35A C36 H36F 74.7 . . ? C35B C36 H36F 110.4 . . ? H36A C36 H36F 75.1 . . ? H36B C36 H36F 62.1 . . ? H36C C36 H36F 171.5 . . ? H36D C36 H36F 109.5 . . ? H36E C36 H36F 109.5 . . ? N5 C37A C38 105.0(10) . . ? N5 C37A H37A 110.7 . . ? C38 C37A H37A 110.7 . . ? N5 C37A H37B 110.7 . . ? C38 C37A H37B 110.7 . . ? H37A C37A H37B 108.8 . . ? N5 C37A H38E 120.2 . . ? C38 C37A H38E 35.0 . . ? H37A C37A H38E 75.8 . . ? H37B C37A H38E 123.2 . . ? N5 C37B C38 106.2(10) . . ? N5 C37B H37C 110.5 . . ? C38 C37B H37C 110.5 . . ? N5 C37B H37D 110.5 . . ? C38 C37B H37D 110.5 . . ? H37C C37B H37D 108.7 . . ? C37A C38 C37B 70.8(9) . . ? C37A C38 H38A 109.5 . . ? C37B C38 H38A 179.1 . . ? C37A C38 H38B 109.5 . . ? C37B C38 H38B 71.1 . . ? H38A C38 H38B 109.5 . . ? C37A C38 H38C 109.5 . . ? C37B C38 H38C 69.7 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37A C38 H38D 178.9 . . ? C37B C38 H38D 109.2 . . ? H38A C38 H38D 70.5 . . ? H38B C38 H38D 71.5 . . ? H38C C38 H38D 69.6 . . ? C37A C38 H38E 69.6 . . ? C37B C38 H38E 109.5 . . ? H38A C38 H38E 69.9 . . ? H38B C38 H38E 178.5 . . ? H38C C38 H38E 72.1 . . ? H38D C38 H38E 109.5 . . ? C37A C38 H38F 71.4 . . ? C37B C38 H38F 109.7 . . ? H38A C38 H38F 71.2 . . ? H38B C38 H38F 69.0 . . ? H38C C38 H38F 178.5 . . ? H38D C38 H38F 109.5 . . ? H38E C38 H38F 109.5 . . ? N5 C39A C40 113.8(10) . . ? N5 C39A H39A 108.8 . . ? C40 C39A H39A 108.8 . . ? N5 C39A H39B 108.8 . . ? C40 C39A H39B 108.8 . . ? H39A C39A H39B 107.7 . . ? N5 C39A H40E 128.4 . . ? C40 C39A H40E 35.8 . . ? H39A C39A H40E 73.0 . . ? H39B C39A H40E 119.8 . . ? N5 C39A H40F 125.9 . . ? C40 C39A H40F 35.4 . . ? H39A C39A H40F 122.2 . . ? H39B C39A H40F 73.4 . . ? H40E C39A H40F 59.8 . . ? C40 C39B N5 113.0(10) . . ? C40 C39B H39C 109.0 . . ? N5 C39B H39C 109.0 . . ? C40 C39B H39D 109.0 . . ? N5 C39B H39D 109.0 . . ? H39C C39B H39D 107.8 . . ? C39B C40 C39A 66.5(9) . . ? C39B C40 H40A 175.8 . . ? C39A C40 H40A 109.5 . . ? C39B C40 H40B 73.6 . . ? C39A C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39B C40 H40C 71.6 . . ? C39A C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39B C40 H40D 109.5 . . ? C39A C40 H40D 175.9 . . ? H40A C40 H40D 74.4 . . ? H40B C40 H40D 69.8 . . ? H40C C40 H40D 67.5 . . ? C39B C40 H40E 109.6 . . ? C39A C40 H40E 71.5 . . ? H40A C40 H40E 67.3 . . ? H40B C40 H40E 176.7 . . ? H40C C40 H40E 72.8 . . ? H40D C40 H40E 109.5 . . ? C39B C40 H40F 109.3 . . ? C39A C40 H40F 73.5 . . ? H40A C40 H40F 69.9 . . ? H40B C40 H40F 68.2 . . ? H40C C40 H40F 176.8 . . ? H40D C40 H40F 109.5 . . ? H40E C40 H40F 109.5 . . ? N5 C41A C42 106.3(9) . . ? N5 C41A H41A 110.5 . . ? C42 C41A H41A 110.5 . . ? N5 C41A H41B 110.5 . . ? C42 C41A H41B 110.5 . . ? H41A C41A H41B 108.7 . . ? N5 C41A H42F 126.1 . . ? C42 C41A H42F 35.0 . . ? H41A C41A H42F 117.7 . . ? H41B C41A H42F 76.0 . . ? C42 C41B N5 101.8(11) . . ? C42 C41B H41C 111.4 . . ? N5 C41B H41C 111.4 . . ? C42 C41B H41D 111.4 . . ? N5 C41B H41D 111.4 . . ? H41C C41B H41D 109.3 . . ? C41B C42 C41A 73.2(9) . . ? C41B C42 H42A 171.6 . . ? C41A C42 H42A 109.5 . . ? C41B C42 H42B 62.3 . . ? C41A C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41B C42 H42C 76.4 . . ? C41A C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41B C42 H42D 107.0 . . ? C41A C42 H42D 173.1 . . ? H42A C42 H42D 69.3 . . ? H42B C42 H42D 65.4 . . ? H42C C42 H42D 77.1 . . ? C41B C42 H42E 111.4 . . ? C41A C42 H42E 76.4 . . ? H42A C42 H42E 77.0 . . ? H42B C42 H42E 168.2 . . ? H42C C42 H42E 58.7 . . ? H42D C42 H42E 109.5 . . ? C41B C42 H42F 109.9 . . ? C41A C42 H42F 64.5 . . ? H42A C42 H42F 65.5 . . ? H42B C42 H42F 82.3 . . ? H42C C42 H42F 168.2 . . ? H42D C42 H42F 109.5 . . ? H42E C42 H42F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.901 _refine_diff_density_min -0.926 _refine_diff_density_rms 0.232 _chemical_compound_source 'Sodium Molybdate' _exptl_crystal_recrystallization_method 'Dichloromethane, petroleum ether' #===END data_27sep _database_code_depnum_ccdc_archive 'CCDC 692000' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 N P2, C33 H20 Mo N4 O2 P S5, C2 H3 N' _chemical_formula_sum 'C71 H53 Mo1 N6 O2 P3 S5' _chemical_formula_weight 1371.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.671(5) _cell_length_b 14.423(5) _cell_length_c 17.921(5) _cell_angle_alpha 85.404(5) _cell_angle_beta 87.751(5) _cell_angle_gamma 80.342(5) _cell_volume 3471(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 28.33 _exptl_crystal_description needle _exptl_crystal_colour pink _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.312 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.456 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.959 _exptl_absorpt_correction_T_max 0.970 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX' _diffrn_measurement_method w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22938 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0789 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 28.33 _reflns_number_total 17312 _reflns_number_gt 11996 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART 5.628(Bruker, 2003)' _computing_cell_refinement 'SAINT 6.45(Bruker, 2003)' _computing_data_reduction 'SAINT 6.45(Bruker, 2003)' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Diamond 2.1e, ORTEP' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1053P)^2^+9.8489P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17312 _refine_ls_number_parameters 794 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1027 _refine_ls_R_factor_gt 0.0702 _refine_ls_wR_factor_ref 0.2487 _refine_ls_wR_factor_gt 0.1723 _refine_ls_goodness_of_fit_ref 1.199 _refine_ls_restrained_S_all 1.199 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.46809(3) 0.86671(3) 0.25949(2) 0.02064(13) Uani 1 1 d . . . S1 S 0.49235(10) 0.74219(10) 0.18022(7) 0.0259(3) Uani 1 1 d . . . S2 S 0.52921(10) 0.94902(10) 0.15263(7) 0.0253(3) Uani 1 1 d . . . S3 S 0.50414(9) 0.75069(9) 0.35931(7) 0.0232(3) Uani 1 1 d . . . S4 S 0.59548(10) 0.93172(9) 0.31257(7) 0.0235(3) Uani 1 1 d . . . S5 S 0.35534(9) 1.00660(9) 0.28129(7) 0.0223(3) Uani 1 1 d . . . P1 P 0.29843(10) 0.81124(10) 0.27672(8) 0.0228(3) Uani 1 1 d . . . P2 P 0.78751(10) 0.46684(10) 0.22984(8) 0.0245(3) Uani 1 1 d . . . P3 P 0.99858(10) 0.42167(10) 0.27474(8) 0.0252(3) Uani 1 1 d . . . O1 O 0.5513(3) 1.0947(3) 0.4469(2) 0.0339(9) Uani 1 1 d . . . H1 H 0.5541 1.0633 0.4872 0.051 Uiso 1 1 d R . . O2 O 0.4123(3) 1.0336(3) 0.4381(2) 0.0317(9) Uani 1 1 d . . . N1 N 0.5902(4) 0.6563(4) -0.0025(3) 0.0341(12) Uani 1 1 d . . . N2 N 0.6534(4) 0.9257(4) -0.0349(3) 0.0406(13) Uani 1 1 d . . . N3 N 0.6637(4) 0.6634(4) 0.5219(3) 0.0364(12) Uani 1 1 d . . . N4 N 0.8031(4) 0.8937(4) 0.4402(3) 0.0353(12) Uani 1 1 d . . . N5 N 0.8941(3) 0.4089(3) 0.2457(3) 0.0273(10) Uani 1 1 d . . . N6 N 0.0311(6) 0.2339(7) 0.0491(5) 0.082(3) Uani 1 1 d . . . C1 C 0.5435(4) 0.7797(4) 0.0948(3) 0.0274(11) Uani 1 1 d . . . C2 C 0.5693(4) 0.7134(4) 0.0404(3) 0.0293(12) Uani 1 1 d . . . C3 C 0.5606(4) 0.8713(4) 0.0839(3) 0.0245(11) Uani 1 1 d . . . C4 C 0.6116(4) 0.9017(4) 0.0173(3) 0.0299(12) Uani 1 1 d . . . C5 C 0.6005(4) 0.7788(4) 0.4107(3) 0.0261(11) Uani 1 1 d . . . C6 C 0.6370(4) 0.7150(4) 0.4718(3) 0.0280(12) Uani 1 1 d . . . C7 C 0.6424(4) 0.8558(4) 0.3876(3) 0.0254(11) Uani 1 1 d . . . C8 C 0.7297(4) 0.8763(4) 0.4190(3) 0.0312(12) Uani 1 1 d . . . C9 C 0.4130(4) 1.1103(4) 0.2763(3) 0.0230(10) Uani 1 1 d . . . C10 C 0.4597(4) 1.1400(4) 0.3366(3) 0.0275(12) Uani 1 1 d . . . C11 C 0.4976(4) 1.2236(4) 0.3272(3) 0.0316(12) Uani 1 1 d . . . H11 H 0.5270 1.2437 0.3676 0.038 Uiso 1 1 calc R . . C12 C 0.4933(5) 1.2777(4) 0.2607(4) 0.0369(14) Uani 1 1 d . . . H12 H 0.5182 1.3342 0.2561 0.044 Uiso 1 1 calc R . . C13 C 0.4507(5) 1.2464(4) 0.1998(4) 0.0352(13) Uani 1 1 d . . . H13 H 0.4492 1.2810 0.1537 0.042 Uiso 1 1 calc R . . C14 C 0.4108(4) 1.1646(4) 0.2077(3) 0.0267(11) Uani 1 1 d . . . H14 H 0.3820 1.1450 0.1669 0.032 Uiso 1 1 calc R . . C15 C 0.4707(4) 1.0840(4) 0.4117(3) 0.0265(11) Uani 1 1 d . . . C16 C 0.2217(4) 0.8586(4) 0.3552(3) 0.0239(11) Uani 1 1 d . . . C17 C 0.1164(4) 0.8767(4) 0.3530(4) 0.0313(13) Uani 1 1 d . . . H17 H 0.0846 0.8739 0.3085 0.038 Uiso 1 1 calc R . . C18 C 0.0610(4) 0.8989(5) 0.4183(4) 0.0388(15) Uani 1 1 d . . . H18 H -0.0080 0.9091 0.4172 0.047 Uiso 1 1 calc R . . C19 C 0.1070(5) 0.9057(4) 0.4841(4) 0.0390(15) Uani 1 1 d . . . H19 H 0.0691 0.9203 0.5271 0.047 Uiso 1 1 calc R . . C20 C 0.2102(5) 0.8910(4) 0.4864(3) 0.0335(13) Uani 1 1 d . . . H20 H 0.2415 0.8960 0.5307 0.040 Uiso 1 1 calc R . . C21 C 0.2657(4) 0.8687(4) 0.4220(3) 0.0276(12) Uani 1 1 d . . . H21 H 0.3346 0.8602 0.4236 0.033 Uiso 1 1 calc R . . C22 C 0.3027(4) 0.6839(4) 0.2960(3) 0.0233(10) Uani 1 1 d . . . C23 C 0.2951(4) 0.6445(4) 0.3702(3) 0.0272(11) Uani 1 1 d . . . H23 H 0.2851 0.6834 0.4096 0.033 Uiso 1 1 calc R . . C24 C 0.3025(4) 0.5477(4) 0.3843(3) 0.0311(12) Uani 1 1 d . . . H24 H 0.2948 0.5222 0.4331 0.037 Uiso 1 1 calc R . . C25 C 0.3213(4) 0.4886(4) 0.3264(3) 0.0310(12) Uani 1 1 d . . . H25 H 0.3295 0.4236 0.3366 0.037 Uiso 1 1 calc R . . C26 C 0.3279(4) 0.5264(4) 0.2532(4) 0.0328(13) Uani 1 1 d . . . H26 H 0.3381 0.4869 0.2141 0.039 Uiso 1 1 calc R . . C27 C 0.3193(4) 0.6232(4) 0.2384(3) 0.0306(12) Uani 1 1 d . . . H27 H 0.3246 0.6480 0.1892 0.037 Uiso 1 1 calc R . . C28 C 0.2234(4) 0.8370(4) 0.1933(3) 0.0266(11) Uani 1 1 d . . . C29 C 0.1390(4) 0.7928(4) 0.1863(4) 0.0320(13) Uani 1 1 d . . . H29 H 0.1220 0.7502 0.2244 0.038 Uiso 1 1 calc R . . C30 C 0.0823(5) 0.8127(5) 0.1235(4) 0.0390(14) Uani 1 1 d . . . H30 H 0.0271 0.7837 0.1194 0.047 Uiso 1 1 calc R . . C31 C 0.1066(5) 0.8753(5) 0.0669(4) 0.0407(15) Uani 1 1 d . . . H31 H 0.0664 0.8899 0.0256 0.049 Uiso 1 1 calc R . . C32 C 0.1897(5) 0.9168(5) 0.0706(3) 0.0368(14) Uani 1 1 d . . . H32 H 0.2073 0.9566 0.0307 0.044 Uiso 1 1 calc R . . C33 C 0.2480(4) 0.8990(4) 0.1346(3) 0.0293(12) Uani 1 1 d . . . H33 H 0.3029 0.9286 0.1379 0.035 Uiso 1 1 calc R . . C34 C 0.7828(4) 0.5915(4) 0.2058(3) 0.0290(12) Uani 1 1 d . . . C35 C 0.7870(5) 0.6548(4) 0.2598(3) 0.0335(13) Uani 1 1 d . . . H35 H 0.7829 0.6351 0.3103 0.040 Uiso 1 1 calc R . . C36 C 0.7970(4) 0.7461(5) 0.2387(4) 0.0388(15) Uani 1 1 d . . . H36 H 0.7994 0.7879 0.2753 0.047 Uiso 1 1 calc R . . C37 C 0.8036(5) 0.7771(4) 0.1649(4) 0.0419(15) Uani 1 1 d . . . H37 H 0.8104 0.8394 0.1515 0.050 Uiso 1 1 calc R . . C38 C 0.8000(4) 0.7150(5) 0.1098(4) 0.0411(16) Uani 1 1 d . . . H38 H 0.8040 0.7361 0.0595 0.049 Uiso 1 1 calc R . . C39 C 0.7904(4) 0.6225(5) 0.1294(3) 0.0344(13) Uani 1 1 d . . . H39 H 0.7890 0.5809 0.0925 0.041 Uiso 1 1 calc R . . C40 C 0.7066(4) 0.4511(4) 0.3093(3) 0.0243(11) Uani 1 1 d . . . C41 C 0.6213(4) 0.5158(4) 0.3248(3) 0.0278(12) Uani 1 1 d . . . H41 H 0.6058 0.5710 0.2940 0.033 Uiso 1 1 calc R . . C42 C 0.5605(4) 0.4980(4) 0.3852(4) 0.0357(14) Uani 1 1 d . . . H42 H 0.5040 0.5415 0.3948 0.043 Uiso 1 1 calc R . . C43 C 0.5820(5) 0.4167(4) 0.4318(3) 0.0344(13) Uani 1 1 d . . . H43 H 0.5402 0.4058 0.4726 0.041 Uiso 1 1 calc R . . C44 C 0.6658(5) 0.3517(4) 0.4175(3) 0.0330(13) Uani 1 1 d . . . H44 H 0.6801 0.2965 0.4485 0.040 Uiso 1 1 calc R . . C45 C 0.7281(4) 0.3686(4) 0.3576(3) 0.0279(11) Uani 1 1 d . . . H45 H 0.7849 0.3251 0.3488 0.033 Uiso 1 1 calc R . . C46 C 0.7379(4) 0.4184(4) 0.1538(3) 0.0290(12) Uani 1 1 d . . . C47 C 0.6388(5) 0.4495(5) 0.1327(4) 0.0378(14) Uani 1 1 d . . . H47 H 0.5988 0.4964 0.1578 0.045 Uiso 1 1 calc R . . C48 C 0.6015(5) 0.4102(5) 0.0749(4) 0.0424(16) Uani 1 1 d . . . H48 H 0.5360 0.4306 0.0613 0.051 Uiso 1 1 calc R . . C49 C 0.6601(6) 0.3409(6) 0.0368(4) 0.054(2) Uani 1 1 d . . . H49 H 0.6341 0.3151 -0.0024 0.064 Uiso 1 1 calc R . . C50 C 0.7569(6) 0.3100(6) 0.0568(4) 0.0516(19) Uani 1 1 d . . . H50 H 0.7955 0.2624 0.0315 0.062 Uiso 1 1 calc R . . C51 C 0.7985(5) 0.3492(5) 0.1150(3) 0.0394(15) Uani 1 1 d . . . H51 H 0.8646 0.3297 0.1274 0.047 Uiso 1 1 calc R . . C52 C 0.9895(4) 0.5098(4) 0.3426(3) 0.0269(11) Uani 1 1 d . . . C53 C 0.9209(4) 0.5046(4) 0.4015(3) 0.0284(12) Uani 1 1 d . . . H53 H 0.8856 0.4545 0.4071 0.034 Uiso 1 1 calc R . . C54 C 0.9051(5) 0.5741(5) 0.4518(3) 0.0357(14) Uani 1 1 d . . . H54 H 0.8578 0.5718 0.4903 0.043 Uiso 1 1 calc R . . C55 C 0.9602(5) 0.6472(4) 0.4445(4) 0.0363(14) Uani 1 1 d . . . H55 H 0.9490 0.6944 0.4777 0.044 Uiso 1 1 calc R . . C56 C 1.0310(5) 0.6497(5) 0.3883(4) 0.0409(15) Uani 1 1 d . . . H56 H 1.0684 0.6983 0.3842 0.049 Uiso 1 1 calc R . . C57 C 1.0477(5) 0.5807(4) 0.3373(4) 0.0340(13) Uani 1 1 d . . . H57 H 1.0970 0.5819 0.3002 0.041 Uiso 1 1 calc R . . C58 C 1.0538(4) 0.3097(4) 0.3181(3) 0.0289(12) Uani 1 1 d . . . C59 C 1.1420(4) 0.3009(4) 0.3575(3) 0.0326(13) Uani 1 1 d . . . H59 H 1.1701 0.3541 0.3638 0.039 Uiso 1 1 calc R . . C60 C 1.1873(5) 0.2133(5) 0.3871(3) 0.0370(14) Uani 1 1 d . . . H60 H 1.2462 0.2074 0.4126 0.044 Uiso 1 1 calc R . . C61 C 1.1443(5) 0.1343(4) 0.3784(3) 0.0367(14) Uani 1 1 d . . . H61 H 1.1754 0.0753 0.3974 0.044 Uiso 1 1 calc R . . C62 C 1.0550(4) 0.1426(5) 0.3416(4) 0.0361(14) Uani 1 1 d . . . H62 H 1.0251 0.0898 0.3380 0.043 Uiso 1 1 calc R . . C63 C 1.0111(4) 0.2299(4) 0.3104(3) 0.0288(12) Uani 1 1 d . . . H63 H 0.9529 0.2353 0.2841 0.035 Uiso 1 1 calc R . . C64 C 1.0789(4) 0.4518(4) 0.1979(3) 0.0284(12) Uani 1 1 d . . . C65 C 1.0529(5) 0.5349(5) 0.1534(4) 0.0397(15) Uani 1 1 d . . . H65 H 0.9970 0.5773 0.1664 0.048 Uiso 1 1 calc R . . C66 C 1.1085(5) 0.5560(5) 0.0898(4) 0.0437(16) Uani 1 1 d . . . H66 H 1.0910 0.6125 0.0609 0.052 Uiso 1 1 calc R . . C67 C 1.1917(5) 0.4908(5) 0.0695(3) 0.0372(14) Uani 1 1 d . . . H67 H 1.2290 0.5030 0.0264 0.045 Uiso 1 1 calc R . . C68 C 1.2173(5) 0.4095(5) 0.1138(3) 0.0366(14) Uani 1 1 d . . . H68 H 1.2728 0.3667 0.1005 0.044 Uiso 1 1 calc R . . C69 C 1.1632(4) 0.3893(4) 0.1775(3) 0.0314(12) Uani 1 1 d . . . H69 H 1.1829 0.3338 0.2071 0.038 Uiso 1 1 calc R . . C70 C 0.1425(6) 0.1355(7) 0.1509(5) 0.065(2) Uani 1 1 d . . . H70A H 0.1487 0.1745 0.1909 0.097 Uiso 1 1 calc R . . H70B H 0.2069 0.1142 0.1294 0.097 Uiso 1 1 calc R . . H70C H 0.1133 0.0821 0.1702 0.097 Uiso 1 1 calc R . . C71 C 0.0798(6) 0.1896(7) 0.0940(5) 0.057(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0207(2) 0.0200(2) 0.0206(2) -0.00279(17) 0.00124(16) -0.00117(17) S1 0.0274(6) 0.0260(7) 0.0244(6) -0.0041(5) 0.0036(5) -0.0049(5) S2 0.0285(6) 0.0257(7) 0.0217(6) -0.0028(5) 0.0002(5) -0.0039(5) S3 0.0237(6) 0.0203(6) 0.0253(6) -0.0024(5) 0.0004(5) -0.0030(5) S4 0.0249(6) 0.0219(6) 0.0233(6) -0.0033(5) -0.0012(5) -0.0020(5) S5 0.0239(6) 0.0178(6) 0.0250(6) -0.0054(5) 0.0004(5) -0.0015(5) P1 0.0227(6) 0.0207(7) 0.0240(6) -0.0039(5) 0.0015(5) -0.0001(5) P2 0.0218(6) 0.0250(7) 0.0263(6) -0.0037(6) -0.0004(5) -0.0013(5) P3 0.0217(6) 0.0238(7) 0.0287(7) -0.0032(6) 0.0023(5) 0.0002(5) O1 0.035(2) 0.040(2) 0.029(2) -0.0026(18) -0.0053(17) -0.0128(19) O2 0.032(2) 0.041(2) 0.0237(19) -0.0019(17) -0.0006(16) -0.0105(18) N1 0.042(3) 0.040(3) 0.024(2) -0.021(2) 0.006(2) -0.009(2) N2 0.046(3) 0.053(4) 0.025(2) -0.007(2) 0.004(2) -0.014(3) N3 0.036(3) 0.036(3) 0.038(3) 0.005(2) -0.006(2) -0.010(2) N4 0.030(2) 0.047(3) 0.031(3) -0.007(2) -0.007(2) -0.009(2) N5 0.021(2) 0.029(2) 0.033(2) -0.010(2) 0.0031(19) -0.0035(18) N6 0.057(5) 0.106(7) 0.088(6) -0.009(5) -0.016(4) -0.018(5) C1 0.024(2) 0.029(3) 0.030(3) -0.003(2) -0.001(2) -0.004(2) C2 0.024(2) 0.038(3) 0.027(3) 0.007(2) -0.005(2) -0.012(2) C3 0.015(2) 0.031(3) 0.026(2) 0.007(2) 0.0008(19) -0.003(2) C4 0.035(3) 0.042(3) 0.013(2) -0.006(2) -0.002(2) -0.006(3) C5 0.023(2) 0.017(2) 0.034(3) 0.001(2) -0.001(2) 0.006(2) C6 0.025(3) 0.033(3) 0.025(3) -0.003(2) -0.004(2) 0.000(2) C7 0.021(2) 0.028(3) 0.026(3) -0.005(2) 0.002(2) -0.003(2) C8 0.034(3) 0.027(3) 0.030(3) 0.001(2) 0.004(2) -0.002(2) C9 0.024(2) 0.019(2) 0.024(2) -0.006(2) -0.001(2) 0.002(2) C10 0.029(3) 0.030(3) 0.024(2) -0.010(2) 0.002(2) -0.002(2) C11 0.038(3) 0.025(3) 0.035(3) -0.010(2) -0.004(3) -0.009(2) C12 0.040(3) 0.023(3) 0.049(4) -0.007(3) -0.006(3) -0.008(3) C13 0.045(3) 0.026(3) 0.034(3) -0.001(2) -0.004(3) -0.006(3) C14 0.034(3) 0.018(2) 0.029(3) -0.003(2) -0.005(2) -0.004(2) C15 0.029(3) 0.028(3) 0.022(2) -0.007(2) -0.002(2) -0.001(2) C16 0.015(2) 0.022(3) 0.033(3) -0.003(2) 0.006(2) -0.0004(19) C17 0.013(2) 0.028(3) 0.052(4) -0.013(3) 0.009(2) 0.000(2) C18 0.027(3) 0.034(3) 0.055(4) -0.006(3) 0.016(3) -0.006(3) C19 0.041(3) 0.030(3) 0.044(3) -0.009(3) 0.018(3) 0.000(3) C20 0.043(3) 0.023(3) 0.032(3) -0.003(2) 0.011(3) -0.003(3) C21 0.025(2) 0.028(3) 0.027(3) -0.003(2) 0.007(2) 0.003(2) C22 0.023(2) 0.020(2) 0.029(3) -0.001(2) -0.001(2) -0.009(2) C23 0.027(3) 0.028(3) 0.027(3) -0.003(2) -0.002(2) -0.006(2) C24 0.037(3) 0.028(3) 0.028(3) 0.003(2) -0.001(2) -0.006(2) C25 0.029(3) 0.024(3) 0.040(3) -0.002(2) -0.001(2) -0.004(2) C26 0.029(3) 0.029(3) 0.042(3) -0.013(3) 0.001(2) -0.004(2) C27 0.029(3) 0.032(3) 0.029(3) -0.006(2) 0.005(2) -0.001(2) C28 0.021(2) 0.028(3) 0.033(3) -0.012(2) -0.001(2) -0.006(2) C29 0.018(2) 0.034(3) 0.045(3) -0.005(3) -0.008(2) -0.006(2) C30 0.036(3) 0.039(4) 0.046(4) -0.005(3) -0.007(3) -0.015(3) C31 0.044(4) 0.045(4) 0.033(3) -0.005(3) -0.020(3) -0.004(3) C32 0.040(3) 0.043(4) 0.031(3) -0.006(3) -0.013(3) -0.014(3) C33 0.033(3) 0.028(3) 0.026(3) 0.005(2) -0.009(2) -0.003(2) C34 0.021(2) 0.034(3) 0.031(3) 0.002(2) -0.002(2) -0.005(2) C35 0.037(3) 0.029(3) 0.034(3) -0.005(2) 0.005(3) -0.002(3) C36 0.017(2) 0.036(3) 0.061(4) -0.006(3) 0.017(3) 0.002(2) C37 0.045(4) 0.021(3) 0.057(4) 0.005(3) 0.004(3) -0.002(3) C38 0.029(3) 0.042(4) 0.049(4) 0.017(3) 0.002(3) -0.004(3) C39 0.034(3) 0.038(3) 0.032(3) 0.004(3) -0.006(2) -0.008(3) C40 0.027(2) 0.020(2) 0.027(3) -0.004(2) -0.002(2) -0.004(2) C41 0.027(3) 0.019(3) 0.035(3) -0.002(2) 0.005(2) 0.001(2) C42 0.028(3) 0.031(3) 0.049(4) -0.013(3) 0.010(3) -0.005(2) C43 0.039(3) 0.035(3) 0.032(3) -0.012(3) 0.012(3) -0.013(3) C44 0.042(3) 0.030(3) 0.027(3) 0.001(2) -0.001(3) -0.010(3) C45 0.023(2) 0.029(3) 0.032(3) -0.004(2) -0.002(2) -0.004(2) C46 0.030(3) 0.027(3) 0.030(3) -0.001(2) -0.001(2) -0.007(2) C47 0.030(3) 0.049(4) 0.037(3) -0.002(3) -0.003(3) -0.012(3) C48 0.044(4) 0.051(4) 0.037(3) -0.002(3) -0.008(3) -0.021(3) C49 0.069(5) 0.066(5) 0.035(3) -0.004(3) -0.004(3) -0.037(4) C50 0.062(5) 0.052(5) 0.043(4) -0.015(3) 0.006(4) -0.011(4) C51 0.052(4) 0.038(4) 0.028(3) -0.015(3) 0.005(3) -0.004(3) C52 0.023(2) 0.022(3) 0.034(3) -0.002(2) 0.001(2) 0.001(2) C53 0.021(2) 0.039(3) 0.027(3) -0.005(2) -0.003(2) -0.007(2) C54 0.033(3) 0.042(4) 0.031(3) -0.008(3) 0.001(2) 0.001(3) C55 0.040(3) 0.028(3) 0.039(3) -0.010(3) 0.003(3) 0.005(3) C56 0.046(4) 0.026(3) 0.052(4) -0.007(3) 0.007(3) -0.010(3) C57 0.034(3) 0.029(3) 0.040(3) -0.004(3) 0.004(3) -0.010(2) C58 0.027(3) 0.032(3) 0.025(3) -0.004(2) 0.001(2) 0.003(2) C59 0.033(3) 0.033(3) 0.028(3) -0.003(2) 0.002(2) 0.004(2) C60 0.032(3) 0.042(4) 0.032(3) -0.004(3) 0.002(2) 0.006(3) C61 0.052(4) 0.029(3) 0.023(3) 0.001(2) 0.007(3) 0.009(3) C62 0.031(3) 0.036(3) 0.040(3) -0.004(3) 0.005(3) -0.001(3) C63 0.027(3) 0.017(2) 0.041(3) -0.002(2) 0.005(2) 0.000(2) C64 0.031(3) 0.033(3) 0.023(2) -0.006(2) 0.000(2) -0.008(2) C65 0.031(3) 0.040(4) 0.043(3) 0.005(3) 0.007(3) 0.002(3) C66 0.042(4) 0.047(4) 0.039(3) 0.004(3) 0.003(3) -0.003(3) C67 0.037(3) 0.048(4) 0.029(3) -0.009(3) 0.004(3) -0.010(3) C68 0.032(3) 0.043(4) 0.035(3) -0.016(3) 0.011(3) -0.004(3) C69 0.033(3) 0.031(3) 0.029(3) -0.008(2) 0.002(2) 0.001(2) C70 0.060(5) 0.072(6) 0.060(5) -0.020(5) 0.012(4) -0.001(4) C71 0.048(4) 0.071(6) 0.056(5) -0.021(4) -0.002(4) -0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 S1 2.3507(15) . ? Mo1 S3 2.3570(15) . ? Mo1 S2 2.3702(15) . ? Mo1 S5 2.3739(14) . ? Mo1 S4 2.3744(15) . ? Mo1 P1 2.5773(17) . ? S1 C1 1.742(6) . ? S2 C3 1.725(6) . ? S3 C5 1.756(6) . ? S4 C7 1.736(6) . ? S5 C9 1.799(6) . ? P1 C28 1.824(6) . ? P1 C16 1.828(5) . ? P1 C22 1.832(5) . ? P2 N5 1.578(5) . ? P2 C46 1.786(6) . ? P2 C40 1.792(5) . ? P2 C34 1.806(6) . ? P3 N5 1.583(5) . ? P3 C58 1.794(6) . ? P3 C64 1.799(6) . ? P3 C52 1.815(6) . ? O1 C15 1.328(7) . ? O1 H1 0.8200 . ? O2 C15 1.226(7) . ? N1 C2 1.163(7) . ? N2 C4 1.137(7) . ? N3 C6 1.149(8) . ? N4 C8 1.159(8) . ? N6 C71 1.148(12) . ? C1 C3 1.377(8) . ? C1 C2 1.414(8) . ? C3 C4 1.435(7) . ? C5 C7 1.362(8) . ? C5 C6 1.422(8) . ? C7 C8 1.423(8) . ? C9 C14 1.403(8) . ? C9 C10 1.405(7) . ? C10 C11 1.387(8) . ? C10 C15 1.512(8) . ? C11 C12 1.369(9) . ? C11 H11 0.9300 . ? C12 C13 1.397(9) . ? C12 H12 0.9300 . ? C13 C14 1.375(8) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C16 C21 1.391(8) . ? C16 C17 1.420(7) . ? C17 C18 1.398(8) . ? C17 H17 0.9300 . ? C18 C19 1.376(10) . ? C18 H18 0.9300 . ? C19 C20 1.393(9) . ? C19 H19 0.9300 . ? C20 C21 1.385(7) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C27 1.396(7) . ? C22 C23 1.410(8) . ? C23 C24 1.386(8) . ? C23 H23 0.9300 . ? C24 C25 1.385(8) . ? C24 H24 0.9300 . ? C25 C26 1.385(9) . ? C25 H25 0.9300 . ? C26 C27 1.386(8) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C33 1.393(8) . ? C28 C29 1.424(7) . ? C29 C30 1.375(9) . ? C29 H29 0.9300 . ? C30 C31 1.372(10) . ? C30 H30 0.9300 . ? C31 C32 1.377(9) . ? C31 H31 0.9300 . ? C32 C33 1.405(8) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.392(8) . ? C34 C39 1.412(8) . ? C35 C36 1.369(9) . ? C35 H35 0.9300 . ? C36 C37 1.366(10) . ? C36 H36 0.9300 . ? C37 C38 1.392(10) . ? C37 H37 0.9300 . ? C38 C39 1.378(9) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.399(7) . ? C40 C45 1.411(8) . ? C41 C42 1.373(8) . ? C41 H41 0.9300 . ? C42 C43 1.380(9) . ? C42 H42 0.9300 . ? C43 C44 1.383(9) . ? C43 H43 0.9300 . ? C44 C45 1.377(8) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 C51 1.397(8) . ? C46 C47 1.411(8) . ? C47 C48 1.373(9) . ? C47 H47 0.9300 . ? C48 C49 1.380(11) . ? C48 H48 0.9300 . ? C49 C50 1.376(11) . ? C49 H49 0.9300 . ? C50 C51 1.407(10) . ? C50 H50 0.9300 . ? C51 H51 0.9300 . ? C52 C53 1.391(7) . ? C52 C57 1.392(8) . ? C53 C54 1.386(8) . ? C53 H53 0.9300 . ? C54 C55 1.390(9) . ? C54 H54 0.9300 . ? C55 C56 1.372(9) . ? C55 H55 0.9300 . ? C56 C57 1.389(9) . ? C56 H56 0.9300 . ? C57 H57 0.9300 . ? C58 C63 1.394(8) . ? C58 C59 1.403(8) . ? C59 C60 1.384(9) . ? C59 H59 0.9300 . ? C60 C61 1.389(10) . ? C60 H60 0.9300 . ? C61 C62 1.392(9) . ? C61 H61 0.9300 . ? C62 C63 1.386(8) . ? C62 H62 0.9300 . ? C63 H63 0.9300 . ? C64 C65 1.388(9) . ? C64 C69 1.396(8) . ? C65 C66 1.387(9) . ? C65 H65 0.9300 . ? C66 C67 1.404(9) . ? C66 H66 0.9300 . ? C67 C68 1.365(10) . ? C67 H67 0.9300 . ? C68 C69 1.374(8) . ? C68 H68 0.9300 . ? C69 H69 0.9300 . ? C70 C71 1.449(13) . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Mo1 S3 86.75(5) . . ? S1 Mo1 S2 82.27(5) . . ? S3 Mo1 S2 147.06(5) . . ? S1 Mo1 S5 140.53(5) . . ? S3 Mo1 S5 118.87(5) . . ? S2 Mo1 S5 88.05(5) . . ? S1 Mo1 S4 125.72(5) . . ? S3 Mo1 S4 82.54(5) . . ? S2 Mo1 S4 79.02(5) . . ? S5 Mo1 S4 89.21(5) . . ? S1 Mo1 P1 79.89(5) . . ? S3 Mo1 P1 80.34(5) . . ? S2 Mo1 P1 127.47(5) . . ? S5 Mo1 P1 76.05(5) . . ? S4 Mo1 P1 148.15(5) . . ? C1 S1 Mo1 109.3(2) . . ? C3 S2 Mo1 108.48(19) . . ? C5 S3 Mo1 108.70(19) . . ? C7 S4 Mo1 108.15(19) . . ? C9 S5 Mo1 113.41(17) . . ? C28 P1 C16 107.3(2) . . ? C28 P1 C22 102.6(3) . . ? C16 P1 C22 102.0(2) . . ? C28 P1 Mo1 113.06(18) . . ? C16 P1 Mo1 114.87(18) . . ? C22 P1 Mo1 115.68(17) . . ? N5 P2 C46 108.1(3) . . ? N5 P2 C40 109.7(3) . . ? C46 P2 C40 106.5(3) . . ? N5 P2 C34 115.5(3) . . ? C46 P2 C34 107.7(3) . . ? C40 P2 C34 109.0(3) . . ? N5 P3 C58 106.9(3) . . ? N5 P3 C64 110.8(3) . . ? C58 P3 C64 107.8(3) . . ? N5 P3 C52 113.1(2) . . ? C58 P3 C52 108.9(3) . . ? C64 P3 C52 109.1(3) . . ? C15 O1 H1 109.5 . . ? P2 N5 P3 140.8(3) . . ? C3 C1 C2 122.7(5) . . ? C3 C1 S1 119.0(4) . . ? C2 C1 S1 118.3(4) . . ? N1 C2 C1 177.7(6) . . ? C1 C3 C4 120.3(5) . . ? C1 C3 S2 120.8(4) . . ? C4 C3 S2 118.7(4) . . ? N2 C4 C3 178.9(6) . . ? C7 C5 C6 122.5(5) . . ? C7 C5 S3 119.4(4) . . ? C6 C5 S3 117.8(4) . . ? N3 C6 C5 178.0(6) . . ? C5 C7 C8 123.3(5) . . ? C5 C7 S4 120.9(4) . . ? C8 C7 S4 115.7(4) . . ? N4 C8 C7 175.9(6) . . ? C14 C9 C10 118.4(5) . . ? C14 C9 S5 117.4(4) . . ? C10 C9 S5 124.2(4) . . ? C11 C10 C9 119.1(5) . . ? C11 C10 C15 118.3(5) . . ? C9 C10 C15 122.6(5) . . ? C12 C11 C10 122.4(6) . . ? C12 C11 H11 118.8 . . ? C10 C11 H11 118.8 . . ? C11 C12 C13 118.6(6) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? C14 C13 C12 120.4(6) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C9 121.1(5) . . ? C13 C14 H14 119.5 . . ? C9 C14 H14 119.5 . . ? O2 C15 O1 122.7(5) . . ? O2 C15 C10 124.3(5) . . ? O1 C15 C10 113.0(5) . . ? C21 C16 C17 118.0(5) . . ? C21 C16 P1 119.7(4) . . ? C17 C16 P1 121.9(4) . . ? C18 C17 C16 119.5(6) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C19 C18 C17 120.9(6) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 120.2(6) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C21 C20 C19 119.3(6) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C20 C21 C16 122.0(5) . . ? C20 C21 H21 119.0 . . ? C16 C21 H21 119.0 . . ? C27 C22 C23 118.3(5) . . ? C27 C22 P1 120.9(4) . . ? C23 C22 P1 120.6(4) . . ? C24 C23 C22 120.1(5) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C25 C24 C23 120.5(5) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C26 120.0(6) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C25 C26 C27 119.9(5) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C26 C27 C22 121.1(5) . . ? C26 C27 H27 119.4 . . ? C22 C27 H27 119.4 . . ? C33 C28 C29 118.4(5) . . ? C33 C28 P1 121.0(4) . . ? C29 C28 P1 120.5(5) . . ? C30 C29 C28 120.4(6) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C31 C30 C29 120.3(6) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 120.9(6) . . ? C30 C31 H31 119.5 . . ? C32 C31 H31 119.5 . . ? C31 C32 C33 119.8(6) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C28 C33 C32 120.0(6) . . ? C28 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C35 C34 C39 119.1(6) . . ? C35 C34 P2 122.1(5) . . ? C39 C34 P2 118.1(5) . . ? C36 C35 C34 120.2(6) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C37 C36 C35 121.3(6) . . ? C37 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C36 C37 C38 119.7(6) . . ? C36 C37 H37 120.2 . . ? C38 C37 H37 120.2 . . ? C39 C38 C37 120.4(6) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C38 C39 C34 119.4(6) . . ? C38 C39 H39 120.3 . . ? C34 C39 H39 120.3 . . ? C41 C40 C45 118.2(5) . . ? C41 C40 P2 123.1(4) . . ? C45 C40 P2 118.7(4) . . ? C42 C41 C40 120.2(5) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C43 121.1(5) . . ? C41 C42 H42 119.5 . . ? C43 C42 H42 119.5 . . ? C42 C43 C44 119.7(5) . . ? C42 C43 H43 120.1 . . ? C44 C43 H43 120.1 . . ? C45 C44 C43 120.0(6) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C40 120.7(5) . . ? C44 C45 H45 119.6 . . ? C40 C45 H45 119.6 . . ? C51 C46 C47 120.0(6) . . ? C51 C46 P2 119.3(5) . . ? C47 C46 P2 120.7(5) . . ? C48 C47 C46 119.8(6) . . ? C48 C47 H47 120.1 . . ? C46 C47 H47 120.1 . . ? C47 C48 C49 120.7(7) . . ? C47 C48 H48 119.6 . . ? C49 C48 H48 119.6 . . ? C50 C49 C48 120.1(7) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C49 C50 C51 121.0(7) . . ? C49 C50 H50 119.5 . . ? C51 C50 H50 119.5 . . ? C46 C51 C50 118.3(7) . . ? C46 C51 H51 120.8 . . ? C50 C51 H51 120.8 . . ? C53 C52 C57 120.1(5) . . ? C53 C52 P3 117.2(4) . . ? C57 C52 P3 122.7(4) . . ? C54 C53 C52 119.9(6) . . ? C54 C53 H53 120.1 . . ? C52 C53 H53 120.1 . . ? C53 C54 C55 119.9(5) . . ? C53 C54 H54 120.1 . . ? C55 C54 H54 120.1 . . ? C56 C55 C54 120.0(6) . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C55 C56 C57 120.9(6) . . ? C55 C56 H56 119.6 . . ? C57 C56 H56 119.6 . . ? C56 C57 C52 119.1(6) . . ? C56 C57 H57 120.5 . . ? C52 C57 H57 120.5 . . ? C63 C58 C59 119.5(6) . . ? C63 C58 P3 119.9(4) . . ? C59 C58 P3 120.6(5) . . ? C60 C59 C58 120.2(6) . . ? C60 C59 H59 119.9 . . ? C58 C59 H59 119.9 . . ? C59 C60 C61 119.7(6) . . ? C59 C60 H60 120.2 . . ? C61 C60 H60 120.2 . . ? C60 C61 C62 120.7(6) . . ? C60 C61 H61 119.7 . . ? C62 C61 H61 119.7 . . ? C63 C62 C61 119.6(6) . . ? C63 C62 H62 120.2 . . ? C61 C62 H62 120.2 . . ? C62 C63 C58 120.3(6) . . ? C62 C63 H63 119.8 . . ? C58 C63 H63 119.8 . . ? C65 C64 C69 118.4(5) . . ? C65 C64 P3 120.0(4) . . ? C69 C64 P3 121.3(5) . . ? C66 C65 C64 121.3(6) . . ? C66 C65 H65 119.3 . . ? C64 C65 H65 119.3 . . ? C65 C66 C67 119.1(7) . . ? C65 C66 H66 120.4 . . ? C67 C66 H66 120.4 . . ? C68 C67 C66 119.3(6) . . ? C68 C67 H67 120.4 . . ? C66 C67 H67 120.4 . . ? C67 C68 C69 121.7(6) . . ? C67 C68 H68 119.2 . . ? C69 C68 H68 119.2 . . ? C68 C69 C64 120.2(6) . . ? C68 C69 H69 119.9 . . ? C64 C69 H69 119.9 . . ? C71 C70 H70A 109.5 . . ? C71 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C71 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? N6 C71 C70 178.7(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.902 _refine_diff_density_min -0.910 _refine_diff_density_rms 0.179 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.210 -0.074 0.807 172 35 ' ' 2 0.118 0.701 0.530 9 0 ' ' 3 0.789 0.074 0.193 172 35 ' ' 4 0.882 0.299 0.470 9 0 ' ' _platon_squeeze_details ; ;