# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_6 #TrackingRef 'compounds_1-7.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; '{[Mn(bipy)2(SCN)][Mn(bipy)](AsS4)}2' ; _chemical_name_common {[Mn(bipy)2(SCN)][Mn(bipy)](AsS4)}2 _chemical_melting_point 'not measured' _chemical_formula_moiety {[Mn(bipy)2(SCN)][Mn(bipy)](AsS4)}2 _chemical_formula_sum 'C62 H48 As2 Mn4 N14 S10' _chemical_formula_weight 1679.34 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8914(14) _cell_length_b 10.6839(18) _cell_length_c 19.448(3) _cell_angle_alpha 77.252(13) _cell_angle_beta 86.528(13) _cell_angle_gamma 71.081(12) _cell_volume 1704.5(5) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 6 _cell_measurement_theta_max 15 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 2.045 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.7714 _exptl_absorpt_correction_T_max 0.9992 _exptl_absorpt_process_details 'Psi (Rigaku WinAFC)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6868 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0838 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6328 _reflns_number_gt 4250 _reflns_threshold_expression >2sigma(I) _computing_data_collection WinAFC _computing_cell_refinement WinAFC _computing_data_reduction 'CrystalStructure Version 3.10' _computing_structure_solution 'Siemens SHELXTL^TM^ 5' _computing_structure_refinement 'Siemens SHELXTL^TM^ 5' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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^)+(0.0714P)^2^+14.9713P] 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 6328 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1147 _refine_ls_R_factor_gt 0.0626 _refine_ls_wR_factor_ref 0.1853 _refine_ls_wR_factor_gt 0.1416 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.002 _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 As1 As 0.55179(3) 0.43658(3) 0.371097(16) 0.02192(8) Uani 1 1 d . . . Mn1 Mn 0.72199(5) 0.32602(5) 0.19072(2) 0.03125(14) Uani 1 1 d . . . Mn2 Mn 0.32206(5) 0.64815(4) 0.46225(2) 0.02554(13) Uani 1 1 d . . . S1 S 0.43957(9) 0.65025(7) 0.33219(4) 0.0298(2) Uani 1 1 d . . . S2 S 0.55099(9) 0.30871(7) 0.29891(4) 0.0305(2) Uani 1 1 d . . . S3 S 0.78705(8) 0.39386(7) 0.41090(4) 0.0299(2) Uani 1 1 d . . . S4 S 0.40930(8) 0.39112(7) 0.46319(4) 0.0262(2) Uani 1 1 d . . . S41 S 0.62127(19) -0.05009(11) 0.11839(7) 0.0903(5) Uani 1 1 d . . . N11 N 0.8289(3) 0.3571(3) 0.07628(15) 0.0431(9) Uani 1 1 d . . . N21 N 0.9667(3) 0.1801(3) 0.22654(15) 0.0390(9) Uani 1 1 d . . . N22 N 0.8691(3) 0.4478(2) 0.21826(13) 0.0303(7) Uani 1 1 d . . . N31 N 0.0628(3) 0.7432(2) 0.42728(13) 0.0260(7) Uani 1 1 d . . . N32 N 0.2662(3) 0.8739(2) 0.43891(13) 0.0278(7) Uani 1 1 d . . . N41 N 0.6464(4) 0.1724(3) 0.16167(16) 0.0539(10) Uani 1 1 d . . . C11 C 0.9571(5) 0.2674(4) 0.0549(2) 0.0593(14) Uani 1 1 d . . . H11B H 1.0103 0.1891 0.0871 0.071 Uiso 1 1 calc R . . C12 C 1.0133(5) 0.2869(5) -0.0134(2) 0.0673(15) Uani 1 1 d . . . H12A H 1.1019 0.2228 -0.0270 0.081 Uiso 1 1 calc R . . C13 C 0.9356(5) 0.4018(5) -0.0598(2) 0.0790(16) Uani 1 1 d . . . H13A H 0.9724 0.4189 -0.1056 0.095 Uiso 1 1 calc R . . C14 C 0.8033(5) 0.4921(4) -0.03894(19) 0.0645(14) Uani 1 1 d . . . H14A H 0.7465 0.5692 -0.0711 0.077 Uiso 1 1 calc R . . C15 C 0.7532(4) 0.4683(3) 0.03110(18) 0.0467(11) Uani 1 1 d . . . C16 C 0.6074(4) 0.5639(3) 0.05729(17) 0.0451(10) Uani 1 1 d . . . C17 C 0.5282(6) 0.6909(4) 0.0171(2) 0.0713(16) Uani 1 1 d . . . H17A H 0.5640 0.7204 -0.0276 0.086 Uiso 1 1 calc R . . C18 C 0.3959(6) 0.7721(4) 0.0445(2) 0.0734(17) Uani 1 1 d . . . H18A H 0.3388 0.8565 0.0181 0.088 Uiso 1 1 calc R . . C19 C 0.3492(5) 0.7268(4) 0.1114(2) 0.0626(15) Uani 1 1 d . . . H19A H 0.2609 0.7807 0.1312 0.075 Uiso 1 1 calc R . . C21 C 1.0079(5) 0.0464(3) 0.2302(2) 0.0511(13) Uani 1 1 d . . . H21B H 0.9297 0.0082 0.2257 0.061 Uiso 1 1 calc R . . C22 C 1.1644(5) -0.0356(4) 0.2405(2) 0.0620(15) Uani 1 1 d . . . H22A H 1.1903 -0.1283 0.2439 0.074 Uiso 1 1 calc R . . C23 C 1.2809(5) 0.0193(4) 0.2456(2) 0.0597(15) Uani 1 1 d . . . H23A H 1.3868 -0.0352 0.2508 0.072 Uiso 1 1 calc R . . C24 C 1.2407(4) 0.1553(4) 0.2431(2) 0.0540(13) Uani 1 1 d . . . H24A H 1.3185 0.1948 0.2461 0.065 Uiso 1 1 calc R . . C25 C 1.0787(4) 0.2341(3) 0.23602(17) 0.0373(10) Uani 1 1 d . . . C26 C 1.0223(3) 0.3814(3) 0.23719(17) 0.0343(9) Uani 1 1 d . . . C27 C 1.1199(4) 0.4426(4) 0.2592(2) 0.0469(12) Uani 1 1 d . . . H27A H 1.2243 0.3926 0.2730 0.056 Uiso 1 1 calc R . . C28 C 1.0622(4) 0.5772(4) 0.2606(2) 0.0519(12) Uani 1 1 d . . . H28A H 1.1269 0.6208 0.2742 0.062 Uiso 1 1 calc R . . C29 C 0.9051(4) 0.6470(3) 0.24117(19) 0.0476(11) Uani 1 1 d . . . H29A H 0.8620 0.7383 0.2423 0.057 Uiso 1 1 calc R . . C31 C -0.0345(4) 0.6748(3) 0.42012(18) 0.0378(10) Uani 1 1 d . . . H31A H 0.0033 0.5807 0.4327 0.045 Uiso 1 1 calc R . . C32 C -0.1883(4) 0.7363(4) 0.39505(19) 0.0474(12) Uani 1 1 d . . . H32A H -0.2527 0.6850 0.3908 0.057 Uiso 1 1 calc R . . C33 C -0.2440(4) 0.8749(4) 0.3764(2) 0.0512(13) Uani 1 1 d . . . H33A H -0.3461 0.9191 0.3578 0.061 Uiso 1 1 calc R . . C34 C -0.1478(4) 0.9480(3) 0.38563(19) 0.0411(11) Uani 1 1 d . . . H34A H -0.1851 1.0421 0.3749 0.049 Uiso 1 1 calc R . . C35 C 0.0070(4) 0.8788(3) 0.41132(17) 0.0327(9) Uani 1 1 d . . . C36 C 0.1156(3) 0.9531(3) 0.42152(15) 0.0258(9) Uani 1 1 d . . . C37 C 0.0719(4) 1.0916(3) 0.41110(18) 0.0388(10) Uani 1 1 d . . . H37A H -0.0335 1.1442 0.4010 0.047 Uiso 1 1 calc R . . C38 C 0.1832(4) 1.1516(3) 0.41555(19) 0.0423(11) Uani 1 1 d . . . H38A H 0.1537 1.2454 0.4088 0.051 Uiso 1 1 calc R . . C39 C 0.3387(4) 1.0745(3) 0.4300(2) 0.0471(11) Uani 1 1 d . . . H39A H 0.4174 1.1141 0.4305 0.056 Uiso 1 1 calc R . . C41 C 0.6367(4) 0.0797(4) 0.14450(18) 0.0459(12) Uani 1 1 d . . . C110 C 0.4354(4) 0.5999(4) 0.1490(2) 0.0491(12) Uani 1 1 d . . . H11A H 0.4032 0.5698 0.1943 0.059 Uiso 1 1 calc R . . N12 N 0.5629(3) 0.5188(3) 0.12270(14) 0.0395(9) Uani 1 1 d . . . C210 C 0.8127(4) 0.5798(3) 0.22008(18) 0.0404(10) Uani 1 1 d . . . H21A H 0.7076 0.6279 0.2066 0.048 Uiso 1 1 calc R . . C310 C 0.3739(4) 0.9356(3) 0.44371(18) 0.0361(10) Uani 1 1 d . . . H31B H 0.4775 0.8819 0.4570 0.043 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 As1 0.01823(12) 0.01930(11) 0.02729(14) -0.00858(10) 0.00275(11) -0.00279(9) Mn1 0.0292(2) 0.0366(2) 0.0292(2) -0.01039(18) 0.00346(19) -0.01051(17) Mn2 0.0224(2) 0.01724(17) 0.0342(2) -0.00808(16) 0.00103(18) -0.00102(15) S1 0.0295(4) 0.0205(3) 0.0324(4) -0.0028(3) 0.0014(3) -0.0005(3) S2 0.0319(3) 0.0341(3) 0.0311(4) -0.0173(3) 0.0069(3) -0.0124(3) S3 0.0182(3) 0.0322(3) 0.0378(4) -0.0120(3) 0.0037(3) -0.0037(3) S4 0.0233(3) 0.0216(3) 0.0351(4) -0.0091(3) 0.0064(3) -0.0079(2) S41 0.1435(10) 0.0628(5) 0.0862(8) -0.0369(5) 0.0171(8) -0.0511(6) N11 0.0498(15) 0.0535(14) 0.0303(14) -0.0111(12) 0.0033(12) -0.0214(12) N21 0.0375(14) 0.0380(13) 0.0388(15) -0.0104(11) 0.0070(12) -0.0079(11) N22 0.0323(12) 0.0364(12) 0.0233(12) -0.0093(10) 0.0072(10) -0.0118(10) N31 0.0242(11) 0.0260(10) 0.0256(12) -0.0036(9) 0.0045(10) -0.0070(9) N32 0.0268(11) 0.0182(10) 0.0369(14) -0.0053(9) 0.0031(11) -0.0060(9) N41 0.0624(17) 0.0667(15) 0.0506(16) -0.0321(12) 0.0107(14) -0.0336(12) C11 0.055(2) 0.086(2) 0.0371(19) -0.0242(18) 0.0201(17) -0.0189(19) C12 0.060(2) 0.099(3) 0.050(2) -0.0331(19) 0.0256(19) -0.029(2) C13 0.097(3) 0.125(3) 0.041(2) -0.036(2) 0.036(2) -0.066(2) C14 0.082(2) 0.102(3) 0.0198(18) -0.0032(18) 0.0065(18) -0.0504(19) C15 0.0639(18) 0.0589(16) 0.0322(17) -0.0154(14) 0.0068(15) -0.0371(13) C16 0.0682(19) 0.0510(15) 0.0276(16) -0.0102(13) -0.0115(15) -0.0313(13) C17 0.096(3) 0.072(2) 0.045(2) 0.010(2) -0.011(2) -0.039(2) C18 0.087(3) 0.059(2) 0.065(3) 0.003(2) -0.026(2) -0.018(2) C19 0.064(3) 0.047(2) 0.064(2) -0.0196(18) -0.012(2) 0.0071(19) C21 0.057(2) 0.0360(16) 0.056(2) -0.0121(16) 0.0067(19) -0.0096(15) C22 0.072(3) 0.050(2) 0.044(2) -0.0102(18) 0.010(2) 0.005(2) C23 0.043(2) 0.057(2) 0.058(2) -0.0098(19) 0.0040(19) 0.0101(19) C24 0.0284(17) 0.071(2) 0.054(2) -0.0165(19) 0.0074(17) -0.0041(17) C25 0.0223(14) 0.0481(17) 0.0348(17) -0.0054(14) 0.0062(13) -0.0056(13) C26 0.0264(14) 0.0460(15) 0.0320(16) -0.0084(13) 0.0043(13) -0.0141(12) C27 0.0277(14) 0.0647(19) 0.053(2) -0.0097(17) 0.0040(15) -0.0231(13) C28 0.0541(17) 0.0716(19) 0.046(2) -0.0175(16) 0.0101(16) -0.0405(14) C29 0.0580(19) 0.0445(15) 0.050(2) -0.0198(14) 0.0160(17) -0.0253(14) C31 0.0331(15) 0.0401(15) 0.0441(18) -0.0153(13) 0.0084(14) -0.0141(12) C32 0.0322(15) 0.069(2) 0.047(2) -0.0141(16) 0.0036(15) -0.0228(14) C33 0.0105(13) 0.071(2) 0.062(2) -0.0070(19) 0.0057(15) -0.0044(14) C34 0.0233(15) 0.0374(16) 0.053(2) -0.0016(15) -0.0016(15) -0.0018(13) C35 0.0315(15) 0.0293(14) 0.0336(16) -0.0059(12) 0.0071(13) -0.0064(12) C36 0.0212(13) 0.0191(12) 0.0285(15) 0.0007(11) 0.0048(12) 0.0006(10) C37 0.0388(17) 0.0192(13) 0.0487(19) -0.0049(13) -0.0043(15) 0.0031(13) C38 0.0572(19) 0.0203(13) 0.050(2) -0.0096(13) 0.0028(17) -0.0122(13) C39 0.0528(18) 0.0314(14) 0.064(2) -0.0109(14) -0.0030(17) -0.0215(12) C41 0.0530(19) 0.0619(19) 0.0237(16) -0.0079(15) 0.0002(15) -0.0205(15) C110 0.0448(19) 0.0570(19) 0.047(2) -0.0172(15) -0.0039(16) -0.0130(15) N12 0.0410(14) 0.0444(13) 0.0338(14) -0.0080(11) -0.0043(12) -0.0138(11) C210 0.0363(16) 0.0453(16) 0.0410(18) -0.0163(14) 0.0156(14) -0.0131(13) C310 0.0253(14) 0.0317(14) 0.0521(19) -0.0102(13) 0.0024(14) -0.0099(11) _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 As1 S3 2.1457(9) . ? As1 S1 2.1521(8) . ? As1 S2 2.1659(10) . ? As1 S4 2.1884(9) . ? Mn1 N41 2.153(4) . ? Mn1 N12 2.265(2) . ? Mn1 N21 2.270(3) . ? Mn1 N22 2.277(3) . ? Mn1 N11 2.364(3) . ? Mn1 S2 2.5291(10) . ? Mn2 N32 2.245(2) . ? Mn2 N31 2.275(2) . ? Mn2 S3 2.5947(10) 2_666 ? Mn2 S4 2.5964(9) . ? Mn2 S1 2.6758(10) . ? Mn2 S4 2.7359(10) 2_666 ? S3 Mn2 2.5947(10) 2_666 ? S4 Mn2 2.7359(10) 2_666 ? S41 C41 1.625(5) . ? N11 C15 1.315(4) . ? N11 C11 1.342(5) . ? N21 C21 1.341(5) . ? N21 C25 1.342(5) . ? N22 C210 1.343(4) . ? N22 C26 1.347(4) . ? N31 C31 1.331(5) . ? N31 C35 1.340(4) . ? N32 C310 1.344(5) . ? N32 C36 1.348(3) . ? N41 C41 1.143(5) . ? C11 C12 1.385(5) . ? C11 H11B 0.9300 . ? C12 C13 1.355(6) . ? C12 H12A 0.9300 . ? C13 C14 1.364(6) . ? C13 H13A 0.9300 . ? C14 C15 1.402(5) . ? C14 H14A 0.9300 . ? C15 C16 1.508(5) . ? C16 N12 1.341(4) . ? C16 C17 1.388(5) . ? C17 C18 1.373(6) . ? C17 H17A 0.9300 . ? C18 C19 1.374(6) . ? C18 H18A 0.9300 . ? C19 C110 1.385(5) . ? C19 H19A 0.9300 . ? C21 C22 1.382(5) . ? C21 H21B 0.9300 . ? C22 C23 1.363(7) . ? C22 H22A 0.9300 . ? C23 C24 1.370(6) . ? C23 H23A 0.9300 . ? C24 C25 1.410(4) . ? C24 H24A 0.9300 . ? C25 C26 1.494(5) . ? C26 C27 1.378(6) . ? C27 C28 1.367(5) . ? C27 H27A 0.9300 . ? C28 C29 1.383(5) . ? C28 H28A 0.9300 . ? C29 C210 1.382(6) . ? C29 H29A 0.9300 . ? C31 C32 1.377(4) . ? C31 H31A 0.9300 . ? C32 C33 1.371(5) . ? C32 H32A 0.9300 . ? C33 C34 1.374(6) . ? C33 H33A 0.9300 . ? C34 C35 1.396(4) . ? C34 H34A 0.9300 . ? C35 C36 1.480(5) . ? C36 C37 1.374(4) . ? C37 C38 1.357(6) . ? C37 H37A 0.9300 . ? C38 C39 1.370(5) . ? C38 H38A 0.9300 . ? C39 C310 1.380(4) . ? C39 H39A 0.9300 . ? C110 N12 1.336(4) . ? C110 H11A 0.9300 . ? C210 H21A 0.9300 . ? C310 H31B 0.9300 . ? 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 As1 S1 111.54(4) . . ? S3 As1 S2 111.11(3) . . ? S1 As1 S2 115.50(3) . . ? S3 As1 S4 105.82(3) . . ? S1 As1 S4 102.84(3) . . ? S2 As1 S4 109.24(4) . . ? N41 Mn1 N12 102.50(11) . . ? N41 Mn1 N21 93.23(11) . . ? N12 Mn1 N21 151.18(11) . . ? N41 Mn1 N22 164.26(10) . . ? N12 Mn1 N22 88.76(10) . . ? N21 Mn1 N22 72.11(10) . . ? N41 Mn1 N11 86.42(12) . . ? N12 Mn1 N11 70.67(9) . . ? N21 Mn1 N11 86.62(10) . . ? N22 Mn1 N11 87.02(11) . . ? N41 Mn1 S2 87.75(9) . . ? N12 Mn1 S2 99.98(7) . . ? N21 Mn1 S2 104.68(7) . . ? N22 Mn1 S2 101.24(7) . . ? N11 Mn1 S2 167.57(8) . . ? N32 Mn2 N31 72.25(9) . . ? N32 Mn2 S3 100.86(7) . 2_666 ? N31 Mn2 S3 85.78(6) . 2_666 ? N32 Mn2 S4 168.24(7) . . ? N31 Mn2 S4 108.77(7) . . ? S3 Mn2 S4 90.90(3) 2_666 . ? N32 Mn2 S1 88.13(7) . . ? N31 Mn2 S1 95.64(7) . . ? S3 Mn2 S1 170.89(3) 2_666 . ? S4 Mn2 S1 80.11(3) . . ? N32 Mn2 S4 92.01(7) . 2_666 ? N31 Mn2 S4 157.05(7) . 2_666 ? S3 Mn2 S4 80.82(3) 2_666 2_666 ? S4 Mn2 S4 90.09(3) . 2_666 ? S1 Mn2 S4 100.54(3) . 2_666 ? As1 S1 Mn2 84.86(3) . . ? As1 S2 Mn1 116.75(4) . . ? As1 S3 Mn2 88.62(3) . 2_666 ? As1 S4 Mn2 86.11(3) . . ? As1 S4 Mn2 84.22(3) . 2_666 ? Mn2 S4 Mn2 89.91(3) . 2_666 ? C15 N11 C11 119.1(3) . . ? C15 N11 Mn1 116.7(2) . . ? C11 N11 Mn1 124.1(2) . . ? C21 N21 C25 119.2(3) . . ? C21 N21 Mn1 123.1(3) . . ? C25 N21 Mn1 117.2(2) . . ? C210 N22 C26 117.3(3) . . ? C210 N22 Mn1 124.9(2) . . ? C26 N22 Mn1 117.7(2) . . ? C31 N31 C35 118.4(2) . . ? C31 N31 Mn2 125.09(18) . . ? C35 N31 Mn2 116.4(2) . . ? C310 N32 C36 117.6(2) . . ? C310 N32 Mn2 123.59(17) . . ? C36 N32 Mn2 118.8(2) . . ? C41 N41 Mn1 166.9(3) . . ? N11 C11 C12 122.6(3) . . ? N11 C11 H11B 118.7 . . ? C12 C11 H11B 118.7 . . ? C13 C12 C11 118.3(4) . . ? C13 C12 H12A 120.9 . . ? C11 C12 H12A 120.9 . . ? C12 C13 C14 119.6(4) . . ? C12 C13 H13A 120.2 . . ? C14 C13 H13A 120.2 . . ? C13 C14 C15 119.7(3) . . ? C13 C14 H14A 120.1 . . ? C15 C14 H14A 120.1 . . ? N11 C15 C14 120.7(3) . . ? N11 C15 C16 117.0(3) . . ? C14 C15 C16 122.3(3) . . ? N12 C16 C17 122.7(3) . . ? N12 C16 C15 115.2(3) . . ? C17 C16 C15 122.1(3) . . ? C18 C17 C16 118.7(4) . . ? C18 C17 H17A 120.7 . . ? C16 C17 H17A 120.7 . . ? C17 C18 C19 119.1(4) . . ? C17 C18 H18A 120.5 . . ? C19 C18 H18A 120.5 . . ? C18 C19 C110 119.1(4) . . ? C18 C19 H19A 120.4 . . ? C110 C19 H19A 120.4 . . ? N21 C21 C22 121.2(4) . . ? N21 C21 H21B 119.4 . . ? C22 C21 H21B 119.4 . . ? C23 C22 C21 120.2(4) . . ? C23 C22 H22A 119.9 . . ? C21 C22 H22A 119.9 . . ? C22 C23 C24 119.4(4) . . ? C22 C23 H23A 120.3 . . ? C24 C23 H23A 120.3 . . ? C23 C24 C25 118.5(4) . . ? C23 C24 H24A 120.7 . . ? C25 C24 H24A 120.7 . . ? N21 C25 C24 121.2(3) . . ? N21 C25 C26 116.3(3) . . ? C24 C25 C26 122.5(4) . . ? N22 C26 C27 122.8(3) . . ? N22 C26 C25 115.5(3) . . ? C27 C26 C25 121.6(3) . . ? C28 C27 C26 119.6(3) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? C27 C28 C29 118.3(4) . . ? C27 C28 H28A 120.8 . . ? C29 C28 H28A 120.8 . . ? C210 C29 C28 119.4(3) . . ? C210 C29 H29A 120.3 . . ? C28 C29 H29A 120.3 . . ? N31 C31 C32 123.3(3) . . ? N31 C31 H31A 118.4 . . ? C32 C31 H31A 118.4 . . ? C33 C32 C31 118.4(4) . . ? C33 C32 H32A 120.8 . . ? C31 C32 H32A 120.8 . . ? C32 C33 C34 119.4(3) . . ? C32 C33 H33A 120.3 . . ? C34 C33 H33A 120.3 . . ? C33 C34 C35 119.1(3) . . ? C33 C34 H34A 120.5 . . ? C35 C34 H34A 120.5 . . ? N31 C35 C34 121.3(3) . . ? N31 C35 C36 117.6(3) . . ? C34 C35 C36 121.0(3) . . ? N32 C36 C37 121.5(3) . . ? N32 C36 C35 114.5(2) . . ? C37 C36 C35 124.0(3) . . ? C38 C37 C36 119.8(3) . . ? C38 C37 H37A 120.1 . . ? C36 C37 H37A 120.1 . . ? C37 C38 C39 120.2(3) . . ? C37 C38 H38A 119.9 . . ? C39 C38 H38A 119.9 . . ? C38 C39 C310 117.4(4) . . ? C38 C39 H39A 121.3 . . ? C310 C39 H39A 121.3 . . ? N41 C41 S41 178.7(3) . . ? N12 C110 C19 122.6(4) . . ? N12 C110 H11A 118.7 . . ? C19 C110 H11A 118.7 . . ? C110 N12 C16 117.8(3) . . ? C110 N12 Mn1 121.6(2) . . ? C16 N12 Mn1 120.0(2) . . ? N22 C210 C29 122.5(3) . . ? N22 C210 H21A 118.8 . . ? C29 C210 H21A 118.8 . . ? N32 C310 C39 123.4(3) . . ? N32 C310 H31B 118.3 . . ? C39 C310 H31B 118.3 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.131 _refine_diff_density_min -0.950 _refine_diff_density_rms 0.164 _database_code_depnum_ccdc_archive 'CCDC 819897' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compound_7 #TrackingRef 'compounds_1-7.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; {[Mn(2-2'bipy)2(SCN)]2(AsIII2S6)} ; _chemical_name_common {[Mn(2-2'bipy)2(SCN)]2(AsIII2S6)} _chemical_melting_point 'not measured' _chemical_formula_moiety 'C42 H32 As2 Mn2 N10 S8' _chemical_formula_sum 'C42 H32 As2 Mn2 N10 S8' _chemical_formula_weight 1192.98 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 '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_space_group_name_hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.7703(12) _cell_length_b 10.0337(13) _cell_length_c 13.5967(17) _cell_angle_alpha 81.461(10) _cell_angle_beta 89.595(11) _cell_angle_gamma 87.716(11) _cell_volume 1182.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 6 _cell_measurement_theta_max 15 _exptl_crystal_description chunk _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 598 _exptl_absorpt_coefficient_mu 2.321 _exptl_absorpt_correction_type Psi-scan _exptl_absorpt_correction_T_min 0.5744 _exptl_absorpt_correction_T_max 0.9899 _exptl_absorpt_process_details 'Psi (Rigaku WinAFC)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC7R' _diffrn_measurement_method \w-2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4764 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0755 _diffrn_reflns_limit_h_min -3 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4391 _reflns_number_gt 3010 _reflns_threshold_expression >2sigma(I) _computing_data_collection WinAFC _computing_cell_refinement WinAFC _computing_data_reduction 'CrystalStructure Version 3.10' _computing_structure_solution 'Siemens SHELXTL^TM^ 5' _computing_structure_refinement 'Siemens SHELXTL^TM^ 5' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Siemens SHELXTL^TM^ 5' _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^)+(0.0430P)^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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4391 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1132 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 As1 As 0.49936(4) 0.87388(3) 0.39802(2) 0.03546(10) Uani 1 1 d . . . Mn1 Mn 0.64868(6) 0.65828(5) 0.23755(4) 0.03111(13) Uani 1 1 d . . . S1 S 0.53544(11) 0.65734(8) 0.41408(6) 0.0373(2) Uani 1 1 d . . . S2 S 0.32188(10) 0.87461(9) 0.52283(7) 0.0380(2) Uani 1 1 d . . . S3 S 0.28776(10) 1.08092(9) 0.51684(7) 0.0383(2) Uani 1 1 d . . . S31 S 0.22592(13) 0.92790(11) 0.06266(8) 0.0674(3) Uani 1 1 d . . . N11 N 0.7454(3) 0.6125(3) 0.08707(19) 0.0338(7) Uani 1 1 d . . . N12 N 0.5668(3) 0.4556(3) 0.21191(18) 0.0326(7) Uani 1 1 d . . . N21 N 0.8696(3) 0.5578(3) 0.30862(19) 0.0365(8) Uani 1 1 d . . . N22 N 0.8171(3) 0.8206(3) 0.24287(19) 0.0366(8) Uani 1 1 d . . . N31 N 0.4720(4) 0.7894(3) 0.1626(2) 0.0503(9) Uani 1 1 d . . . C11 C 0.8343(4) 0.6942(4) 0.0272(3) 0.0474(11) Uani 1 1 d . . . H11B H 0.8615 0.7748 0.0471 0.057 Uiso 1 1 calc R . . C12 C 0.8873(5) 0.6641(4) -0.0628(3) 0.0549(12) Uani 1 1 d . . . H12A H 0.9513 0.7221 -0.1018 0.066 Uiso 1 1 calc R . . C13 C 0.8448(4) 0.5485(4) -0.0936(3) 0.0546(12) Uani 1 1 d . . . H13A H 0.8780 0.5279 -0.1549 0.066 Uiso 1 1 calc R . . C14 C 0.7537(4) 0.4627(4) -0.0352(2) 0.0451(11) Uani 1 1 d . . . H14A H 0.7264 0.3824 -0.0554 0.054 Uiso 1 1 calc R . . C15 C 0.7013(4) 0.4973(3) 0.0564(2) 0.0326(9) Uani 1 1 d . . . C16 C 0.6040(4) 0.4106(3) 0.1252(2) 0.0306(8) Uani 1 1 d . . . C17 C 0.5481(4) 0.2897(3) 0.1048(3) 0.0426(10) Uani 1 1 d . . . H17A H 0.5715 0.2603 0.0445 0.051 Uiso 1 1 calc R . . C18 C 0.4600(4) 0.2143(3) 0.1720(3) 0.0503(11) Uani 1 1 d . . . H18A H 0.4238 0.1332 0.1582 0.060 Uiso 1 1 calc R . . C19 C 0.4237(4) 0.2588(3) 0.2617(3) 0.0452(11) Uani 1 1 d . . . H19A H 0.3632 0.2091 0.3090 0.054 Uiso 1 1 calc R . . C21 C 0.8900(4) 0.4265(4) 0.3439(3) 0.0461(11) Uani 1 1 d . . . H21B H 0.8122 0.3693 0.3347 0.055 Uiso 1 1 calc R . . C22 C 1.0195(4) 0.3714(4) 0.3929(3) 0.0530(12) Uani 1 1 d . . . H22A H 1.0289 0.2794 0.4162 0.064 Uiso 1 1 calc R . . C23 C 1.1337(4) 0.4549(4) 0.4065(3) 0.0577(13) Uani 1 1 d . . . H23A H 1.2226 0.4202 0.4392 0.069 Uiso 1 1 calc R . . C24 C 1.1173(4) 0.5913(4) 0.3717(3) 0.0544(12) Uani 1 1 d . . . H24A H 1.1956 0.6487 0.3794 0.065 Uiso 1 1 calc R . . C25 C 0.9810(4) 0.6416(4) 0.3249(2) 0.0375(9) Uani 1 1 d . . . C26 C 0.9490(4) 0.7885(3) 0.2913(2) 0.0361(9) Uani 1 1 d . . . C27 C 1.0453(4) 0.8872(4) 0.3112(3) 0.0571(12) Uani 1 1 d . . . H27A H 1.1352 0.8630 0.3463 0.069 Uiso 1 1 calc R . . C28 C 1.0079(5) 1.0217(4) 0.2790(3) 0.0656(13) Uani 1 1 d . . . H28A H 1.0727 1.0885 0.2912 0.079 Uiso 1 1 calc R . . C29 C 0.8737(5) 1.0545(4) 0.2289(3) 0.0563(12) Uani 1 1 d . . . H29A H 0.8444 1.1442 0.2073 0.068 Uiso 1 1 calc R . . C31 C 0.3704(4) 0.8477(3) 0.1219(2) 0.0374(9) Uani 1 1 d . . . C110 C 0.4812(4) 0.3793(3) 0.2775(3) 0.0404(10) Uani 1 1 d . . . H11A H 0.4590 0.4095 0.3376 0.049 Uiso 1 1 calc R . . C210 C 0.7829(4) 0.9519(3) 0.2112(3) 0.0434(10) Uani 1 1 d . . . H21A H 0.6932 0.9744 0.1755 0.052 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 As1 0.0455(2) 0.02936(17) 0.03172(17) -0.00738(14) -0.00176(16) 0.00675(16) Mn1 0.0324(3) 0.0274(2) 0.0346(3) -0.0098(2) -0.0057(2) 0.0059(2) S1 0.0469(5) 0.0267(4) 0.0388(5) -0.0078(4) 0.0014(4) 0.0044(4) S2 0.0384(5) 0.0328(4) 0.0434(5) -0.0082(4) 0.0007(4) -0.0006(4) S3 0.0368(5) 0.0360(4) 0.0427(5) -0.0098(4) 0.0020(4) 0.0077(4) S31 0.0708(7) 0.0638(6) 0.0651(7) -0.0115(5) -0.0201(6) 0.0390(6) N11 0.0378(16) 0.0295(14) 0.0335(14) -0.0036(12) -0.0005(13) 0.0018(13) N12 0.0334(15) 0.0326(14) 0.0329(14) -0.0089(12) 0.0016(13) -0.0001(13) N21 0.0353(16) 0.0353(15) 0.0374(15) -0.0026(13) -0.0019(14) 0.0086(13) N22 0.0363(16) 0.0386(15) 0.0360(15) -0.0105(12) -0.0040(14) 0.0050(14) N31 0.058(2) 0.0432(17) 0.0510(18) -0.0132(15) -0.0185(17) 0.0131(16) C11 0.055(2) 0.039(2) 0.047(2) -0.0001(17) 0.002(2) 0.0007(19) C12 0.055(2) 0.060(3) 0.044(2) 0.007(2) 0.017(2) 0.001(2) C13 0.058(3) 0.066(3) 0.037(2) -0.0035(19) 0.010(2) 0.014(2) C14 0.049(2) 0.047(2) 0.0396(19) -0.0127(17) 0.0012(18) 0.0126(19) C15 0.0331(18) 0.0340(17) 0.0300(17) -0.0055(14) -0.0057(15) 0.0104(15) C16 0.0289(17) 0.0312(16) 0.0322(17) -0.0085(14) -0.0062(15) 0.0099(14) C17 0.051(2) 0.0374(18) 0.0437(19) -0.0215(15) -0.0053(18) 0.0057(17) C18 0.057(2) 0.0277(18) 0.067(2) -0.0118(18) -0.004(2) -0.0001(18) C19 0.043(2) 0.0361(19) 0.055(2) -0.0028(17) 0.0021(19) -0.0033(18) C21 0.045(2) 0.043(2) 0.049(2) -0.0076(17) -0.0076(19) 0.0154(18) C22 0.052(2) 0.053(2) 0.051(2) -0.0050(19) -0.007(2) 0.029(2) C23 0.037(2) 0.083(3) 0.048(2) -0.003(2) -0.0085(19) 0.031(2) C24 0.030(2) 0.080(3) 0.054(2) -0.014(2) -0.0085(19) 0.012(2) C25 0.0323(19) 0.049(2) 0.0305(17) -0.0079(16) -0.0014(16) 0.0081(17) C26 0.0330(19) 0.0453(19) 0.0309(17) -0.0074(15) 0.0001(16) -0.0046(16) C27 0.043(2) 0.073(3) 0.058(2) -0.015(2) -0.008(2) -0.008(2) C28 0.077(3) 0.056(2) 0.069(3) -0.020(2) 0.007(2) -0.027(2) C29 0.069(3) 0.040(2) 0.061(2) -0.0072(19) 0.010(2) -0.008(2) C31 0.050(2) 0.0287(16) 0.0362(18) -0.0141(14) -0.0043(17) 0.0077(17) C110 0.042(2) 0.0428(19) 0.0379(19) -0.0091(16) 0.0033(17) -0.0024(17) C210 0.051(2) 0.0369(19) 0.042(2) -0.0037(16) 0.0005(19) -0.0025(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 S1 2.1619(9) . ? As1 S2 2.2953(10) . ? As1 S3 2.2990(10) 2_676 ? Mn1 N31 2.152(3) . ? Mn1 N22 2.252(3) . ? Mn1 N12 2.259(3) . ? Mn1 N21 2.299(3) . ? Mn1 N11 2.311(3) . ? Mn1 S1 2.5900(10) . ? S2 S3 2.0694(12) . ? S3 As1 2.2990(10) 2_676 ? S31 C31 1.625(3) . ? N11 C11 1.337(4) . ? N11 C15 1.358(4) . ? N12 C110 1.333(4) . ? N12 C16 1.357(4) . ? N21 C21 1.339(4) . ? N21 C25 1.355(4) . ? N22 C26 1.339(4) . ? N22 C210 1.346(4) . ? N31 C31 1.146(4) . ? C11 C12 1.376(5) . ? C11 H11B 0.9300 . ? C12 C13 1.357(6) . ? C12 H12A 0.9300 . ? C13 C14 1.362(5) . ? C13 H13A 0.9300 . ? C14 C15 1.410(4) . ? C14 H14A 0.9300 . ? C15 C16 1.471(4) . ? C16 C17 1.393(5) . ? C17 C18 1.355(5) . ? C17 H17A 0.9300 . ? C18 C19 1.390(5) . ? C18 H18A 0.9300 . ? C19 C110 1.375(5) . ? C19 H19A 0.9300 . ? C21 C22 1.376(5) . ? C21 H21B 0.9300 . ? C22 C23 1.362(6) . ? C22 H22A 0.9300 . ? C23 C24 1.382(6) . ? C23 H23A 0.9300 . ? C24 C25 1.398(5) . ? C24 H24A 0.9300 . ? C25 C26 1.493(5) . ? C26 C27 1.384(5) . ? C27 C28 1.383(6) . ? C27 H27A 0.9300 . ? C28 C29 1.368(6) . ? C28 H28A 0.9300 . ? C29 C210 1.376(5) . ? C29 H29A 0.9300 . ? C110 H11A 0.9300 . ? C210 H21A 0.9300 . ? 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 As1 S2 96.35(4) . . ? S1 As1 S3 97.53(4) . 2_676 ? S2 As1 S3 99.17(4) . 2_676 ? N31 Mn1 N22 95.77(11) . . ? N31 Mn1 N12 100.31(11) . . ? N22 Mn1 N12 156.81(10) . . ? N31 Mn1 N21 167.60(11) . . ? N22 Mn1 N21 72.10(10) . . ? N12 Mn1 N21 90.62(10) . . ? N31 Mn1 N11 90.84(10) . . ? N22 Mn1 N11 91.48(10) . . ? N12 Mn1 N11 71.79(9) . . ? N21 Mn1 N11 86.99(9) . . ? N31 Mn1 S1 95.37(8) . . ? N22 Mn1 S1 97.58(7) . . ? N12 Mn1 S1 97.44(7) . . ? N21 Mn1 S1 88.95(7) . . ? N11 Mn1 S1 168.43(7) . . ? As1 S1 Mn1 94.66(3) . . ? S3 S2 As1 98.88(4) . . ? S2 S3 As1 99.45(5) . 2_676 ? C11 N11 C15 118.6(3) . . ? C11 N11 Mn1 124.6(2) . . ? C15 N11 Mn1 116.6(2) . . ? C110 N12 C16 118.6(3) . . ? C110 N12 Mn1 122.9(2) . . ? C16 N12 Mn1 118.5(2) . . ? C21 N21 C25 118.0(3) . . ? C21 N21 Mn1 125.2(2) . . ? C25 N21 Mn1 116.4(2) . . ? C26 N22 C210 118.0(3) . . ? C26 N22 Mn1 118.8(2) . . ? C210 N22 Mn1 122.6(2) . . ? C31 N31 Mn1 173.2(3) . . ? N11 C11 C12 122.7(4) . . ? N11 C11 H11B 118.6 . . ? C12 C11 H11B 118.6 . . ? C13 C12 C11 119.0(4) . . ? C13 C12 H12A 120.5 . . ? C11 C12 H12A 120.5 . . ? C12 C13 C14 120.2(4) . . ? C12 C13 H13A 119.9 . . ? C14 C13 H13A 119.9 . . ? C13 C14 C15 119.1(4) . . ? C13 C14 H14A 120.4 . . ? C15 C14 H14A 120.4 . . ? N11 C15 C14 120.2(3) . . ? N11 C15 C16 116.5(3) . . ? C14 C15 C16 123.2(3) . . ? N12 C16 C17 119.9(3) . . ? N12 C16 C15 116.4(3) . . ? C17 C16 C15 123.7(3) . . ? C18 C17 C16 120.5(3) . . ? C18 C17 H17A 119.7 . . ? C16 C17 H17A 119.7 . . ? C17 C18 C19 119.7(3) . . ? C17 C18 H18A 120.1 . . ? C19 C18 H18A 120.1 . . ? C110 C19 C18 117.1(3) . . ? C110 C19 H19A 121.4 . . ? C18 C19 H19A 121.4 . . ? N21 C21 C22 123.7(4) . . ? N21 C21 H21B 118.1 . . ? C22 C21 H21B 118.1 . . ? C23 C22 C21 118.2(4) . . ? C23 C22 H22A 120.9 . . ? C21 C22 H22A 120.9 . . ? C22 C23 C24 120.0(3) . . ? C22 C23 H23A 120.0 . . ? C24 C23 H23A 120.0 . . ? C23 C24 C25 118.9(4) . . ? C23 C24 H24A 120.5 . . ? C25 C24 H24A 120.5 . . ? N21 C25 C24 120.9(3) . . ? N21 C25 C26 116.4(3) . . ? C24 C25 C26 122.7(3) . . ? N22 C26 C27 121.2(3) . . ? N22 C26 C25 115.8(3) . . ? C27 C26 C25 123.0(3) . . ? C28 C27 C26 120.1(4) . . ? C28 C27 H27A 120.0 . . ? C26 C27 H27A 120.0 . . ? C29 C28 C27 118.7(4) . . ? C29 C28 H28A 120.6 . . ? C27 C28 H28A 120.6 . . ? C28 C29 C210 118.4(4) . . ? C28 C29 H29A 120.8 . . ? C210 C29 H29A 120.8 . . ? N31 C31 S31 178.7(3) . . ? N12 C110 C19 124.1(3) . . ? N12 C110 H11A 118.0 . . ? C19 C110 H11A 118.0 . . ? N22 C210 C29 123.5(3) . . ? N22 C210 H21A 118.2 . . ? C29 C210 H21A 118.2 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.104 _refine_diff_density_min -1.185 _refine_diff_density_rms 0.113 _database_code_depnum_ccdc_archive 'CCDC 819898'