# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # 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_c:2012_jf175 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H66 Fe2 Mo2 N8 O6, 2(C F3 O3 S), 2(C2 H3 N)' _chemical_formula_sum 'C62 H72 F6 Fe2 Mo2 N10 O12 S2' _chemical_formula_weight 1631.00 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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' 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' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6964(2) _cell_length_b 20.4165(4) _cell_length_c 29.0322(5) _cell_angle_alpha 91.626(1) _cell_angle_beta 90.650(1) _cell_angle_gamma 96.328(1) _cell_volume 6887.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 82955 _cell_measurement_theta_min 2.04 _cell_measurement_theta_max 27.82 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.330 _exptl_crystal_size_mid 0.173 _exptl_crystal_size_min 0.080 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3328 _exptl_absorpt_coefficient_mu 0.912 _exptl_absorpt_process_details 'STOE X-RED' _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7809 _exptl_absorpt_correction_T_max 0.9336 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -1 -6 0.0410 0 1 5 0.0580 4 -3 0 0.1580 -4 3 0 0.1780 3 -1 7 0.1300 0 7 -1 0.0320 0 -6 1 0.0540 _exptl_special_details ; ? ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 45 _diffrn_source_power 2.25 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_ambient_temperature 100(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 362 frames, detector distance = 115 mm ; _diffrn_reflns_number 77931 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.00 _diffrn_reflns_theta_full 27.00 _diffrn_reflns_av_unetI/netI 0.0737 _diffrn_reflns_av_R_equivalents 0.0651 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 36 _reflns_d_resolution_high 0.783 _reflns_d_resolution_low 10.142 _reflns_special_details 'Friedel pairs have been merged' _reflns_limit_h_min -14 _reflns_limit_h_max 14 _reflns_limit_k_min -26 _reflns_limit_k_max 26 _reflns_limit_l_min 0 _reflns_limit_l_max 37 _reflns_number_total 29954 _reflns_number_gt 21224 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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 fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0916P)^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 0.00480(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 29954 _refine_ls_number_parameters 1872 _refine_ls_number_restraints 221 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1486 _refine_ls_wR_factor_gt 0.1373 _refine_ls_goodness_of_fit_ref 0.990 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.035 _refine_ls_shift/su_mean 0.001 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.631 _refine_diff_density_min -1.325 _refine_diff_density_rms 0.136 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 0.94194(3) 0.79037(2) 0.253586(14) 0.02131(9) Uani 1 1 d . . . Mo2 Mo 0.53269(3) 0.686052(19) 0.261926(14) 0.02118(9) Uani 1 1 d . . . Fe1 Fe 0.71335(5) 0.76938(3) 0.16665(2) 0.02026(13) Uani 1 1 d . . . Fe2 Fe 0.71191(5) 0.78424(3) 0.34684(2) 0.02098(13) Uani 1 1 d . . . O1 O 0.8605(3) 0.77748(18) 0.20057(12) 0.0270(7) Uani 1 1 d . . . O2 O 0.8452(3) 0.77678(18) 0.29872(12) 0.0285(7) Uani 1 1 d . . . O3 O 0.6059(3) 0.71685(17) 0.31385(12) 0.0280(7) Uani 1 1 d . . . O4 O 0.6250(3) 0.70587(17) 0.21587(12) 0.0271(7) Uani 1 1 d . . . O5 O 0.9874(3) 0.87387(18) 0.25768(13) 0.0298(7) Uani 1 1 d . . . O6 O 0.4204(3) 0.73358(18) 0.25476(14) 0.0326(8) Uani 1 1 d . . . N1 N 0.5511(3) 0.7774(2) 0.12650(14) 0.0231(8) Uani 1 1 d . . . N2 N 0.6552(3) 0.8623(2) 0.19327(14) 0.0228(8) Uani 1 1 d . . . N3 N 0.7752(3) 0.8357(2) 0.11172(14) 0.0236(8) Uani 1 1 d . . . N4 N 0.6964(3) 0.6851(2) 0.11793(14) 0.0240(8) Uani 1 1 d . . . N5 N 0.8108(3) 0.8684(2) 0.38563(14) 0.0231(8) Uani 1 1 d . . . N6 N 0.6496(3) 0.8753(2) 0.31699(14) 0.0239(8) Uani 1 1 d . . . N7 N 0.8156(3) 0.7390(2) 0.39901(14) 0.0251(8) Uani 1 1 d . . . N8 N 0.5861(3) 0.8093(2) 0.39772(14) 0.0255(8) Uani 1 1 d . . . C1 C 1.1185(4) 0.7620(3) 0.28620(17) 0.0260(10) Uani 1 1 d . . . C2 C 1.1447(4) 0.7794(3) 0.23996(18) 0.0272(10) Uani 1 1 d . . . C3 C 1.0829(4) 0.7317(3) 0.20998(18) 0.0283(10) Uani 1 1 d . . . C4 C 1.0178(4) 0.6853(3) 0.23751(19) 0.0280(10) Uani 1 1 d . . . C5 C 1.0400(4) 0.7030(3) 0.28450(18) 0.0278(10) Uani 1 1 d . . . C6 C 0.5690(4) 0.5736(2) 0.28081(17) 0.0252(10) Uani 1 1 d . . . C7 C 0.5310(4) 0.5719(2) 0.23396(17) 0.0261(10) Uani 1 1 d . . . C8 C 0.4158(4) 0.5890(2) 0.23388(17) 0.0260(10) Uani 1 1 d . . . C9 C 0.3828(4) 0.5989(2) 0.28011(17) 0.0245(9) Uani 1 1 d . . . C10 C 0.4770(4) 0.5899(2) 0.30914(16) 0.0237(9) Uani 1 1 d . . . C21 C 1.1747(4) 0.7967(3) 0.32770(19) 0.0336(11) Uani 1 1 d . . . H21A H 1.2556 0.7885 0.3292 0.050 Uiso 1 1 calc R . . H21B H 1.1355 0.7802 0.3554 0.050 Uiso 1 1 calc R . . H21C H 1.1700 0.8441 0.3258 0.050 Uiso 1 1 calc R . . C22 C 1.2237(4) 0.8373(3) 0.2270(2) 0.0338(11) Uani 1 1 d . . . H22A H 1.2250 0.8401 0.1934 0.051 Uiso 1 1 calc R . . H22B H 1.3014 0.8327 0.2386 0.051 Uiso 1 1 calc R . . H22C H 1.1973 0.8775 0.2405 0.051 Uiso 1 1 calc R . . C23 C 1.0831(5) 0.7299(4) 0.1587(2) 0.0417(14) Uani 1 1 d . . . H23A H 1.0105 0.7433 0.1471 0.063 Uiso 1 1 calc R . . H23B H 1.0916 0.6851 0.1474 0.063 Uiso 1 1 calc R . . H23C H 1.1473 0.7603 0.1480 0.063 Uiso 1 1 calc R . . C24 C 0.9411(5) 0.6256(3) 0.2197(2) 0.0407(13) Uani 1 1 d . . . H24A H 0.9211 0.5961 0.2451 0.061 Uiso 1 1 calc R . . H24B H 0.9815 0.6023 0.1960 0.061 Uiso 1 1 calc R . . H24C H 0.8707 0.6395 0.2063 0.061 Uiso 1 1 calc R . . C25 C 0.9936(4) 0.6645(3) 0.3247(2) 0.0345(11) Uani 1 1 d . . . H25A H 0.9102 0.6656 0.3261 0.052 Uiso 1 1 calc R . . H25B H 1.0298 0.6840 0.3532 0.052 Uiso 1 1 calc R . . H25C H 1.0106 0.6187 0.3210 0.052 Uiso 1 1 calc R . . C26 C 0.6851(4) 0.5598(3) 0.2983(2) 0.0342(12) Uani 1 1 d . . . H26A H 0.7237 0.5995 0.3139 0.051 Uiso 1 1 calc R . . H26B H 0.7316 0.5472 0.2723 0.051 Uiso 1 1 calc R . . H26C H 0.6757 0.5238 0.3200 0.051 Uiso 1 1 calc R . . C27 C 0.5993(5) 0.5543(3) 0.19334(19) 0.0322(11) Uani 1 1 d . . . H27A H 0.6612 0.5897 0.1884 0.048 Uiso 1 1 calc R . . H27B H 0.5490 0.5484 0.1659 0.048 Uiso 1 1 calc R . . H27C H 0.6325 0.5132 0.1990 0.048 Uiso 1 1 calc R . . C28 C 0.3364(4) 0.5912(3) 0.1929(2) 0.0338(12) Uani 1 1 d . . . H28A H 0.2707 0.5574 0.1955 0.051 Uiso 1 1 calc R . . H28B H 0.3781 0.5829 0.1646 0.051 Uiso 1 1 calc R . . H28C H 0.3089 0.6348 0.1918 0.051 Uiso 1 1 calc R . . C29 C 0.2669(4) 0.6167(3) 0.2941(2) 0.0335(11) Uani 1 1 d . . . H29A H 0.2099 0.5779 0.2903 0.050 Uiso 1 1 calc R . . H29B H 0.2448 0.6518 0.2746 0.050 Uiso 1 1 calc R . . H29C H 0.2701 0.6321 0.3264 0.050 Uiso 1 1 calc R . . C30 C 0.4822(5) 0.5946(3) 0.36112(19) 0.0333(11) Uani 1 1 d . . . H30A H 0.4075 0.6045 0.3728 0.050 Uiso 1 1 calc R . . H30B H 0.5419 0.6298 0.3711 0.050 Uiso 1 1 calc R . . H30C H 0.5004 0.5526 0.3732 0.050 Uiso 1 1 calc R . . C41 C 0.4795(4) 0.8151(2) 0.15666(17) 0.0254(10) Uani 1 1 d . . . H41A H 0.4482 0.7873 0.1819 0.030 Uiso 1 1 calc R . . H41B H 0.4142 0.8289 0.1387 0.030 Uiso 1 1 calc R . . C42 C 0.5788(4) 0.8116(3) 0.08277(17) 0.0272(10) Uani 1 1 d . . . H42A H 0.5167 0.8390 0.0754 0.033 Uiso 1 1 calc R . . H42B H 0.5807 0.7781 0.0575 0.033 Uiso 1 1 calc R . . C43 C 0.4988(4) 0.7095(2) 0.11721(17) 0.0266(10) Uani 1 1 d . . . H43A H 0.4375 0.7091 0.0934 0.032 Uiso 1 1 calc R . . H43B H 0.4637 0.6912 0.1456 0.032 Uiso 1 1 calc R . . C44 C 0.8232(4) 0.9247(2) 0.35472(18) 0.0285(10) Uani 1 1 d . . . H44A H 0.8787 0.9170 0.3302 0.034 Uiso 1 1 calc R . . H44B H 0.8525 0.9655 0.3723 0.034 Uiso 1 1 calc R . . C45 C 0.7476(4) 0.8833(3) 0.42801(17) 0.0279(10) Uani 1 1 d . . . H45A H 0.7615 0.9311 0.4354 0.034 Uiso 1 1 calc R . . H45B H 0.7783 0.8598 0.4540 0.034 Uiso 1 1 calc R . . C46 C 0.9230(4) 0.8468(3) 0.39773(19) 0.0300(11) Uani 1 1 d . . . H46A H 0.9633 0.8781 0.4208 0.036 Uiso 1 1 calc R . . H46B H 0.9713 0.8461 0.3700 0.036 Uiso 1 1 calc R . . C53 C 0.5526(4) 0.8748(2) 0.17628(17) 0.0248(9) Uani 1 1 d . . . C54 C 0.6919(4) 0.8547(2) 0.08449(16) 0.0258(9) Uani 1 1 d . . . C55 C 0.5900(4) 0.6676(2) 0.10076(16) 0.0253(9) Uani 1 1 d . . . C56 C 0.7068(4) 0.9321(2) 0.33365(17) 0.0263(10) Uani 1 1 d . . . C57 C 0.9054(4) 0.7792(3) 0.41709(17) 0.0269(10) Uani 1 1 d . . . C58 C 0.6196(4) 0.8636(2) 0.42358(17) 0.0262(10) Uani 1 1 d . . . C65 C 0.5190(4) 0.9375(3) 0.17641(19) 0.0319(11) Uani 1 1 d . . . H65 H 0.4459 0.9448 0.1642 0.038 Uiso 1 1 calc R . . C66 C 0.5926(5) 0.9894(3) 0.1945(2) 0.0373(12) Uani 1 1 d . . . H66 H 0.5715 1.0331 0.1947 0.045 Uiso 1 1 calc R . . C67 C 0.6977(4) 0.9768(3) 0.2122(2) 0.0330(11) Uani 1 1 d . . . H67 H 0.7499 1.0116 0.2251 0.040 Uiso 1 1 calc R . . C68 C 0.7259(4) 0.9133(2) 0.21087(17) 0.0267(10) Uani 1 1 d . . . H68 H 0.7986 0.9052 0.2230 0.032 Uiso 1 1 calc R . . C69 C 0.7087(5) 0.9096(3) 0.0575(2) 0.0390(13) Uani 1 1 d . . . H69 H 0.6473 0.9231 0.0396 0.047 Uiso 1 1 calc R . . C70 C 0.8172(6) 0.9443(3) 0.0570(2) 0.0432(14) Uani 1 1 d . . . H70 H 0.8312 0.9822 0.0388 0.052 Uiso 1 1 calc R . . C71 C 0.9051(5) 0.9236(3) 0.0833(2) 0.0432(14) Uani 1 1 d . . . H71 H 0.9809 0.9457 0.0825 0.052 Uiso 1 1 calc R . . C72 C 0.8796(4) 0.8703(3) 0.11058(19) 0.0305(11) Uani 1 1 d . . . H72 H 0.9390 0.8572 0.1297 0.037 Uiso 1 1 calc R . . C73 C 0.5650(5) 0.6143(3) 0.07078(18) 0.0316(11) Uani 1 1 d . . . H73 H 0.4887 0.6026 0.0595 0.038 Uiso 1 1 calc R . . C74 C 0.6527(5) 0.5781(3) 0.0574(2) 0.0359(12) Uani 1 1 d . . . H74 H 0.6371 0.5409 0.0370 0.043 Uiso 1 1 calc R . . C75 C 0.7630(5) 0.5964(3) 0.07390(19) 0.0329(11) Uani 1 1 d . . . H75 H 0.8247 0.5727 0.0646 0.039 Uiso 1 1 calc R . . C76 C 0.7816(4) 0.6503(3) 0.10447(18) 0.0285(10) Uani 1 1 d . . . H76 H 0.8572 0.6629 0.1162 0.034 Uiso 1 1 calc R . . C77 C 0.5451(4) 0.8771(3) 0.29903(17) 0.0280(10) Uani 1 1 d . . . H77 H 0.5035 0.8371 0.2878 0.034 Uiso 1 1 calc R . . C78 C 0.4944(4) 0.9356(3) 0.2961(2) 0.0346(12) Uani 1 1 d . . . H78 H 0.4198 0.9354 0.2828 0.042 Uiso 1 1 calc R . . C79 C 0.5533(5) 0.9933(3) 0.3128(2) 0.0374(12) Uani 1 1 d . . . H79 H 0.5201 1.0337 0.3111 0.045 Uiso 1 1 calc R . . C80 C 0.6621(5) 0.9920(3) 0.33215(19) 0.0320(11) Uani 1 1 d . . . H80 H 0.7048 1.0312 0.3441 0.038 Uiso 1 1 calc R . . C81 C 0.7966(4) 0.6781(3) 0.41512(18) 0.0291(10) Uani 1 1 d . . . H81 H 0.7328 0.6496 0.4031 0.035 Uiso 1 1 calc R . . C82 C 0.8656(5) 0.6549(3) 0.44839(19) 0.0347(11) Uani 1 1 d . . . H82 H 0.8505 0.6109 0.4584 0.042 Uiso 1 1 calc R . . C83 C 0.9562(5) 0.6959(3) 0.46687(19) 0.0363(12) Uani 1 1 d . . . H83 H 1.0042 0.6811 0.4901 0.044 Uiso 1 1 calc R . . C84 C 0.9762(5) 0.7594(3) 0.45093(19) 0.0355(12) Uani 1 1 d . . . H84 H 1.0382 0.7889 0.4632 0.043 Uiso 1 1 calc R . . C85 C 0.5423(5) 0.8984(3) 0.44685(19) 0.0336(11) Uani 1 1 d . . . H85 H 0.5678 0.9384 0.4632 0.040 Uiso 1 1 calc R . . C86 C 0.4272(5) 0.8741(3) 0.44601(19) 0.0343(11) Uani 1 1 d . . . H86 H 0.3729 0.8965 0.4625 0.041 Uiso 1 1 calc R . . C87 C 0.3920(4) 0.8165(3) 0.42074(19) 0.0325(11) Uani 1 1 d . . . H87 H 0.3138 0.7980 0.4203 0.039 Uiso 1 1 calc R . . C88 C 0.4734(4) 0.7870(3) 0.39650(17) 0.0272(10) Uani 1 1 d . . . H88 H 0.4490 0.7488 0.3779 0.033 Uiso 1 1 calc R . . Mo3 Mo 0.85949(3) 0.68795(2) 0.756835(15) 0.02605(9) Uani 1 1 d . . . Mo4 Mo 0.48022(3) 0.78693(2) 0.751904(14) 0.02383(9) Uani 1 1 d . . . Fe3 Fe 0.69355(5) 0.76702(3) 0.66310(2) 0.02288(14) Uani 1 1 d . . . Fe4 Fe 0.71507(6) 0.78205(4) 0.84449(3) 0.02786(15) Uani 1 1 d . . . N9 N 0.8538(3) 0.7771(2) 0.62116(14) 0.0259(8) Uani 1 1 d . . . N10 N 0.6756(3) 0.6813(2) 0.61551(14) 0.0259(8) Uani 1 1 d . . . N11 N 0.6485(3) 0.8340(2) 0.60884(14) 0.0254(8) Uani 1 1 d . . . N12 N 0.7870(3) 0.8612(2) 0.68916(14) 0.0256(8) Uani 1 1 d . . . N13 N 0.6421(3) 0.8621(2) 0.88446(15) 0.0301(9) Uani 1 1 d . . . N14 N 0.8000(4) 0.8748(2) 0.81511(15) 0.0339(10) Uani 1 1 d . . . N15 N 0.8530(3) 0.8118(2) 0.89571(14) 0.0277(9) Uani 1 1 d . . . N16 N 0.6027(4) 0.7315(2) 0.89639(15) 0.0328(10) Uani 1 1 d . . . O7 O 0.7742(3) 0.70888(17) 0.71045(12) 0.0293(7) Uani 1 1 d . . . O8 O 0.8067(3) 0.72509(19) 0.80769(13) 0.0340(8) Uani 1 1 d . . . O9 O 0.5720(3) 0.77033(19) 0.79740(13) 0.0327(8) Uani 1 1 d . . . O10 O 0.5541(3) 0.77381(18) 0.69941(12) 0.0294(7) Uani 1 1 d . . . O11 O 0.9946(3) 0.72888(19) 0.74827(14) 0.0374(9) Uani 1 1 d . . . O12 O 0.4728(3) 0.87079(19) 0.75646(13) 0.0325(8) Uani 1 1 d . . . C11 C 0.9137(4) 0.5833(3) 0.7296(2) 0.0323(11) Uani 1 1 d . . . C12 C 0.7915(4) 0.5737(2) 0.73417(19) 0.0290(10) Uani 1 1 d . . . C13 C 0.7653(4) 0.5822(2) 0.78131(19) 0.0282(10) Uani 1 1 d . . . C14 C 0.8723(4) 0.5943(3) 0.80614(18) 0.0295(11) Uani 1 1 d . . . C15 C 0.9628(4) 0.5941(3) 0.7748(2) 0.0323(11) Uani 1 1 d . . . C16 C 0.2919(4) 0.7636(3) 0.78290(19) 0.0301(11) Uani 1 1 d . . . C17 C 0.2738(4) 0.7793(3) 0.73595(18) 0.0288(10) Uani 1 1 d . . . C18 C 0.3140(4) 0.7310(3) 0.70709(19) 0.0297(11) Uani 1 1 d . . . C19 C 0.3583(4) 0.6835(2) 0.73630(18) 0.0284(10) Uani 1 1 d . . . C20 C 0.3422(4) 0.7035(3) 0.78303(18) 0.0289(10) Uani 1 1 d . . . C31 C 0.9802(5) 0.5771(3) 0.6862(2) 0.0411(13) Uani 1 1 d . . . H31A H 1.0424 0.6133 0.6853 0.062 Uiso 1 1 calc R . . H31B H 0.9288 0.5790 0.6595 0.062 Uiso 1 1 calc R . . H31C H 1.0130 0.5349 0.6854 0.062 Uiso 1 1 calc R . . C32 C 0.7050(5) 0.5606(3) 0.6953(2) 0.0362(12) Uani 1 1 d . . . H32A H 0.6370 0.5333 0.7061 0.054 Uiso 1 1 calc R . . H32B H 0.7393 0.5375 0.6698 0.054 Uiso 1 1 calc R . . H32C H 0.6824 0.6026 0.6847 0.054 Uiso 1 1 calc R . . C33 C 0.6497(4) 0.5795(3) 0.8022(2) 0.0338(11) Uani 1 1 d . . . H33A H 0.6318 0.6244 0.8095 0.051 Uiso 1 1 calc R . . H33B H 0.6491 0.5545 0.8305 0.051 Uiso 1 1 calc R . . H33C H 0.5920 0.5578 0.7804 0.051 Uiso 1 1 calc R . . C34 C 0.8827(5) 0.6058(3) 0.8574(2) 0.0400(13) Uani 1 1 d . . . H34A H 0.9641 0.6141 0.8664 0.060 Uiso 1 1 calc R . . H34B H 0.8474 0.5667 0.8729 0.060 Uiso 1 1 calc R . . H34C H 0.8433 0.6440 0.8664 0.060 Uiso 1 1 calc R . . C35 C 1.0898(4) 0.6053(3) 0.7848(2) 0.0448(15) Uani 1 1 d . . . H35A H 1.1029 0.6174 0.8175 0.067 Uiso 1 1 calc R . . H35B H 1.1248 0.6409 0.7659 0.067 Uiso 1 1 calc R . . H35C H 1.1246 0.5648 0.7776 0.067 Uiso 1 1 calc R . . C36 C 0.2504(5) 0.8001(3) 0.8238(2) 0.0387(12) Uani 1 1 d . . . H36A H 0.2755 0.7807 0.8521 0.058 Uiso 1 1 calc R . . H36B H 0.1662 0.7970 0.8228 0.058 Uiso 1 1 calc R . . H36C H 0.2823 0.8465 0.8232 0.058 Uiso 1 1 calc R . . C37 C 0.2193(4) 0.8393(3) 0.7218(2) 0.0357(12) Uani 1 1 d . . . H37A H 0.2184 0.8413 0.6881 0.054 Uiso 1 1 calc R . . H37B H 0.2637 0.8790 0.7350 0.054 Uiso 1 1 calc R . . H37C H 0.1402 0.8365 0.7330 0.054 Uiso 1 1 calc R . . C38 C 0.3136(5) 0.7273(3) 0.65585(19) 0.0366(12) Uani 1 1 d . . . H38A H 0.2569 0.7547 0.6439 0.055 Uiso 1 1 calc R . . H38B H 0.2933 0.6815 0.6452 0.055 Uiso 1 1 calc R . . H38C H 0.3901 0.7433 0.6448 0.055 Uiso 1 1 calc R . . C39 C 0.4105(5) 0.6235(3) 0.7194(2) 0.0375(12) Uani 1 1 d . . . H39A H 0.4920 0.6356 0.7128 0.056 Uiso 1 1 calc R . . H39B H 0.3702 0.6057 0.6913 0.056 Uiso 1 1 calc R . . H39C H 0.4035 0.5902 0.7431 0.056 Uiso 1 1 calc R . . C40 C 0.3723(4) 0.6651(3) 0.8238(2) 0.0356(12) Uani 1 1 d . . . H40A H 0.4549 0.6743 0.8307 0.053 Uiso 1 1 calc R . . H40B H 0.3532 0.6179 0.8169 0.053 Uiso 1 1 calc R . . H40C H 0.3286 0.6780 0.8506 0.053 Uiso 1 1 calc R . . C47 C 0.8819(4) 0.7105(3) 0.61043(18) 0.0285(10) Uani 1 1 d . . . H47A H 0.9166 0.6924 0.6379 0.034 Uiso 1 1 calc R . . H47B H 0.9387 0.7117 0.5854 0.034 Uiso 1 1 calc R . . C48 C 0.8326(4) 0.8125(3) 0.57828(18) 0.0298(10) Uani 1 1 d . . . H48A H 0.8140 0.7797 0.5528 0.036 Uiso 1 1 calc R . . H48B H 0.9041 0.8402 0.5702 0.036 Uiso 1 1 calc R . . C49 C 0.9432(4) 0.8150(2) 0.65078(17) 0.0266(10) Uani 1 1 d . . . H49A H 1.0115 0.8294 0.6323 0.032 Uiso 1 1 calc R . . H49B H 0.9674 0.7870 0.6756 0.032 Uiso 1 1 calc R . . C50 C 0.6457(5) 0.9189(3) 0.8541(2) 0.0348(12) Uani 1 1 d . . . H50A H 0.6310 0.9588 0.8723 0.042 Uiso 1 1 calc R . . H50B H 0.5851 0.9105 0.8299 0.042 Uiso 1 1 calc R . . C51 C 0.7123(4) 0.8791(3) 0.92723(18) 0.0324(11) Uani 1 1 d . . . H51A H 0.6768 0.8539 0.9530 0.039 Uiso 1 1 calc R . . H51B H 0.7118 0.9266 0.9350 0.039 Uiso 1 1 calc R . . C52 C 0.5240(4) 0.8360(3) 0.8968(2) 0.0378(13) Uani 1 1 d . . . H52A H 0.4728 0.8350 0.8693 0.045 Uiso 1 1 calc R . . H52B H 0.4946 0.8650 0.9207 0.045 Uiso 1 1 calc R . . C59 C 0.7740(4) 0.6666(3) 0.59568(18) 0.0302(10) Uani 1 1 d . . . C60 C 0.7368(4) 0.8555(3) 0.58226(17) 0.0277(10) Uani 1 1 d . . . C61 C 0.8938(4) 0.8741(3) 0.67125(18) 0.0278(10) Uani 1 1 d . . . C62 C 0.7610(5) 0.9298(3) 0.83230(19) 0.0352(12) Uani 1 1 d . . . C63 C 0.8355(4) 0.8640(2) 0.92207(18) 0.0295(10) Uani 1 1 d . . . C64 C 0.5239(4) 0.7676(3) 0.91450(19) 0.0337(12) Uani 1 1 d . . . C89 C 0.7769(5) 0.6141(3) 0.56475(19) 0.0356(12) Uani 1 1 d . . . H89 H 0.8473 0.6054 0.5510 0.043 Uiso 1 1 calc R . . C90 C 0.6756(5) 0.5740(3) 0.5539(2) 0.0385(12) Uani 1 1 d . . . H90 H 0.6755 0.5378 0.5326 0.046 Uiso 1 1 calc R . . C91 C 0.5753(5) 0.5879(3) 0.5747(2) 0.0367(12) Uani 1 1 d . . . H91 H 0.5052 0.5608 0.5687 0.044 Uiso 1 1 calc R . . C92 C 0.5786(4) 0.6419(3) 0.60436(18) 0.0299(10) Uani 1 1 d . . . H92 H 0.5086 0.6519 0.6177 0.036 Uiso 1 1 calc R . . C93 C 0.7372(5) 0.9127(3) 0.55742(19) 0.0362(12) Uani 1 1 d . . . H93 H 0.8021 0.9279 0.5397 0.043 Uiso 1 1 calc R . . C94 C 0.6425(5) 0.9470(3) 0.55881(19) 0.0381(12) Uani 1 1 d . . . H94 H 0.6410 0.9862 0.5420 0.046 Uiso 1 1 calc R . . C95 C 0.5492(5) 0.9238(3) 0.5851(2) 0.0379(12) Uani 1 1 d . . . H95 H 0.4817 0.9457 0.5858 0.045 Uiso 1 1 calc R . . C96 C 0.5566(4) 0.8681(3) 0.61007(18) 0.0309(11) Uani 1 1 d . . . H96 H 0.4940 0.8532 0.6291 0.037 Uiso 1 1 calc R . . C97 C 0.9501(4) 0.9372(3) 0.67197(19) 0.0324(11) Uani 1 1 d . . . H97 H 1.0251 0.9450 0.6596 0.039 Uiso 1 1 calc R . . C98 C 0.8977(4) 0.9884(3) 0.6905(2) 0.0369(12) Uani 1 1 d . . . H98 H 0.9354 1.0320 0.6909 0.044 Uiso 1 1 calc R . . C99 C 0.7891(4) 0.9755(3) 0.70860(19) 0.0321(11) Uani 1 1 d . . . H99 H 0.7508 1.0100 0.7217 0.038 Uiso 1 1 calc R . . C100 C 0.7376(4) 0.9112(3) 0.70716(17) 0.0272(10) Uani 1 1 d . . . H100 H 0.6630 0.9024 0.7197 0.033 Uiso 1 1 calc R . . C101 C 0.8249(5) 0.9913(3) 0.8314(2) 0.0462(15) Uani 1 1 d . . . H101 H 0.7956 1.0294 0.8440 0.055 Uiso 1 1 calc R . . C102 C 0.9326(6) 0.9956(3) 0.8116(2) 0.0500(17) Uani 1 1 d . . . H102 H 0.9781 1.0370 0.8101 0.060 Uiso 1 1 calc R . . C103 C 0.9726(5) 0.9394(4) 0.7942(2) 0.0497(17) Uani 1 1 d . . . H103 H 1.0466 0.9417 0.7808 0.060 Uiso 1 1 calc R . . C104 C 0.9049(5) 0.8792(3) 0.7962(2) 0.0388(13) Uani 1 1 d . . . H104 H 0.9332 0.8405 0.7840 0.047 Uiso 1 1 calc R . . C105 C 0.9243(5) 0.9019(3) 0.9460(2) 0.0364(12) Uani 1 1 d . . . H105 H 0.9096 0.9400 0.9634 0.044 Uiso 1 1 calc R . . C106 C 1.0339(5) 0.8832(3) 0.9439(2) 0.0390(13) Uani 1 1 d . . . H106 H 1.0955 0.9074 0.9607 0.047 Uiso 1 1 calc R . . C107 C 1.0527(4) 0.8282(3) 0.9168(2) 0.0346(12) Uani 1 1 d . . . H107 H 1.1272 0.8141 0.9149 0.042 Uiso 1 1 calc R . . C108 C 0.9601(4) 0.7943(3) 0.89270(19) 0.0327(11) Uani 1 1 d . . . H108 H 0.9730 0.7576 0.8734 0.039 Uiso 1 1 calc R . . C109 C 0.4458(5) 0.7428(3) 0.9467(2) 0.0425(14) Uani 1 1 d . . . H109 H 0.3922 0.7698 0.9594 0.051 Uiso 1 1 calc R . . C110 C 0.4459(5) 0.6781(3) 0.9604(2) 0.0451(15) Uani 1 1 d . . . H110 H 0.3911 0.6598 0.9817 0.054 Uiso 1 1 calc R . . C111 C 0.5269(5) 0.6415(3) 0.9425(2) 0.0434(15) Uani 1 1 d . . . H111 H 0.5300 0.5973 0.9515 0.052 Uiso 1 1 calc R . . C112 C 0.6048(5) 0.6700(3) 0.9110(2) 0.0362(12) Uani 1 1 d . . . H112 H 0.6620 0.6446 0.8993 0.043 Uiso 1 1 calc R . . O201 O 0.7340(5) 0.4966(3) 0.4604(2) 0.0748(17) Uani 1 1 d . . . O202 O 0.6862(4) 0.4279(2) 0.39235(18) 0.0523(11) Uani 1 1 d . . . O203 O 0.8519(4) 0.5102(2) 0.39272(16) 0.0466(10) Uani 1 1 d . . . S200 S 0.77213(12) 0.46762(7) 0.41900(5) 0.0394(3) Uani 1 1 d . . . C200 C 0.8618(5) 0.4074(4) 0.4401(2) 0.0464(15) Uani 1 1 d . . . F201 F 0.9059(4) 0.3737(2) 0.40651(16) 0.0637(11) Uani 1 1 d . . . F202 F 0.9504(4) 0.4355(3) 0.46577(15) 0.0707(13) Uani 1 1 d . . . F203 F 0.8039(4) 0.3632(2) 0.46713(16) 0.0687(13) Uani 1 1 d . . . O301 O 0.3192(3) 0.5006(2) 0.08849(13) 0.0380(9) Uani 1 1 d . . . O302 O 0.1646(3) 0.4673(2) 0.03316(14) 0.0388(9) Uani 1 1 d . . . O303 O 0.3176(3) 0.55232(19) 0.01442(13) 0.0335(8) Uani 1 1 d . . . S300 S 0.25227(10) 0.51746(6) 0.04984(4) 0.0273(2) Uani 1 1 d . . . C300 C 0.1700(4) 0.5807(3) 0.0740(2) 0.0354(12) Uani 1 1 d . . . F301 F 0.1055(3) 0.55837(19) 0.10916(14) 0.0515(9) Uani 1 1 d . . . F302 F 0.0987(3) 0.6010(2) 0.04294(15) 0.0601(11) Uani 1 1 d . . . F303 F 0.2382(3) 0.63317(17) 0.08973(13) 0.0458(8) Uani 1 1 d . . . N600 N 0.7392(4) 0.7541(3) 0.00237(17) 0.0397(11) Uani 1 1 d . . . C601 C 0.8190(5) 0.7272(3) -0.00196(19) 0.0352(12) Uani 1 1 d . . . C602 C 0.9196(5) 0.6922(3) -0.0077(2) 0.0441(14) Uani 1 1 d . . . H60A H 0.8953 0.6462 -0.0171 0.066 Uiso 1 1 calc R . . H60B H 0.9628 0.6936 0.0215 0.066 Uiso 1 1 calc R . . H60C H 0.9687 0.7131 -0.0315 0.066 Uiso 1 1 calc R . . N700 N 0.1663(4) 0.6868(3) 0.9176(2) 0.0484(13) Uani 1 1 d . . . C701 C 0.1484(4) 0.6320(3) 0.9237(2) 0.0368(12) Uani 1 1 d . . . C702 C 0.1243(6) 0.5613(3) 0.9306(2) 0.0520(17) Uani 1 1 d . . . H70A H 0.0517 0.5525 0.9470 0.078 Uiso 1 1 calc R . . H70B H 0.1869 0.5462 0.9489 0.078 Uiso 1 1 calc R . . H70C H 0.1182 0.5377 0.9007 0.078 Uiso 1 1 calc R . . N800 N 0.2281(5) 0.6715(3) 0.4179(2) 0.0507(13) Uani 1 1 d . . . C801 C 0.1834(4) 0.6193(3) 0.4197(2) 0.0382(13) Uani 1 1 d . . . C802 C 0.1248(6) 0.5536(4) 0.4218(3) 0.0570(18) Uani 1 1 d . . . H80A H 0.0425 0.5546 0.4156 0.086 Uiso 1 1 calc R . . H80B H 0.1357 0.5365 0.4526 0.086 Uiso 1 1 calc R . . H80C H 0.1565 0.5249 0.3987 0.086 Uiso 1 1 calc R . . N900 N 0.6443(5) 0.7479(3) 0.49980(19) 0.0489(13) Uani 1 1 d U A 1 C901 C 0.5602(10) 0.7204(7) 0.4997(4) 0.045(3) Uani 0.67(2) 1 d PU A 1 C902 C 0.4414(11) 0.6896(8) 0.5035(5) 0.069(4) Uani 0.67(2) 1 d PU A 1 H90A H 0.4065 0.7075 0.5310 0.103 Uiso 0.67(2) 1 calc PR A 1 H90B H 0.4414 0.6418 0.5061 0.103 Uiso 0.67(2) 1 calc PR A 1 H90C H 0.3971 0.6989 0.4761 0.103 Uiso 0.67(2) 1 calc PR A 1 C911 C 0.5384(19) 0.7391(12) 0.5090(8) 0.040(5) Uani 0.33(2) 1 d PU A 2 C912 C 0.415(2) 0.7278(14) 0.5215(9) 0.061(8) Uani 0.33(2) 1 d PU A 2 H91A H 0.4018 0.6882 0.5398 0.091 Uiso 0.33(2) 1 calc PR A 2 H91B H 0.3672 0.7218 0.4933 0.091 Uiso 0.33(2) 1 calc PR A 2 H91C H 0.3938 0.7659 0.5395 0.091 Uiso 0.33(2) 1 calc PR A 2 O401 O 0.1265(8) 0.9256(5) 0.5844(2) 0.078(2) Uani 0.686(5) 1 d PDU B 1 O402 O 0.0675(6) 0.8977(5) 0.5114(3) 0.088(2) Uani 0.686(5) 1 d PDU B 1 O403 O 0.2808(5) 0.9520(4) 0.5364(3) 0.0460(18) Uani 0.686(5) 1 d PDU B 1 S400 S 0.1692(3) 0.91481(17) 0.53895(14) 0.0455(8) Uani 0.686(5) 1 d PDU B 1 C400 C 0.2110(4) 0.8326(2) 0.5462(2) 0.0530(15) Uani 0.686(5) 1 d PDU B 1 F401 F 0.1310(4) 0.7884(3) 0.56295(18) 0.0470(13) Uani 0.686(5) 1 d PDU B 1 F402 F 0.3121(6) 0.8256(5) 0.5659(3) 0.100(2) Uani 0.686(5) 1 d PDU B 1 F403 F 0.2318(7) 0.8053(4) 0.5053(2) 0.085(2) Uani 0.686(5) 1 d PDU B 1 O411 O 0.1710(19) 0.9053(12) 0.5971(3) 0.078(2) Uani 0.314(5) 1 d PDU B 2 O412 O 0.2576(13) 0.9533(7) 0.5226(5) 0.042(4) Uani 0.314(5) 1 d PDU B 2 O413 O 0.2036(14) 0.8440(5) 0.5232(5) 0.055(4) Uani 0.314(5) 1 d PDU B 2 S410 S 0.1917(6) 0.9041(3) 0.5485(2) 0.0344(16) Uani 0.314(5) 1 d PDU B 2 C410 C 0.0911(7) 0.9411(5) 0.5118(3) 0.035(4) Uani 0.314(5) 1 d PDU B 2 F411 F 0.1268(11) 0.9488(7) 0.4686(4) 0.059(3) Uani 0.314(5) 1 d PDU B 2 F412 F 0.0687(11) 1.0006(5) 0.5270(5) 0.062(4) Uani 0.314(5) 1 d PDU B 2 F413 F -0.0105(8) 0.9044(5) 0.5076(4) 0.044(3) Uani 0.314(5) 1 d PDU B 2 S500 S 0.29824(19) 0.90967(11) 0.04194(9) 0.0355(5) Uani 0.60 1 d PDU C 1 O501 O 0.3614(7) 0.9267(4) 0.0840(2) 0.0518(17) Uani 0.60 1 d PDU C 1 O502 O 0.3715(8) 0.8906(5) 0.0058(3) 0.081(2) Uani 0.60 1 d PDU C 1 O503 O 0.2164(6) 0.9537(3) 0.0295(3) 0.0404(17) Uani 0.60 1 d PDU C 1 C500 C 0.2108(4) 0.8345(2) 0.0572(2) 0.0516(14) Uani 0.60 1 d PDU C 1 F501 F 0.1578(9) 0.8524(6) 0.0953(3) 0.104(3) Uani 0.60 1 d PDU C 1 F502 F 0.2733(5) 0.7858(3) 0.0671(2) 0.0404(14) Uani 0.60 1 d PDU C 1 F503 F 0.1432(8) 0.8090(4) 0.0223(3) 0.084(2) Uani 0.60 1 d PDU C 1 S510 S 0.2564(3) 0.90748(18) 0.06605(14) 0.0398(8) Uiso 0.40 1 d PD D 2 O511 O 0.1888(6) 0.9502(3) 0.0417(3) 0.029(3) Uiso 0.40 1 d PD D 2 O512 O 0.2255(9) 0.8954(7) 0.11295(17) 0.086(5) Uiso 0.40 1 d PD D 2 O513 O 0.3781(4) 0.9231(6) 0.0601(4) 0.066(4) Uiso 0.40 1 d PD D 2 C510 C 0.2274(6) 0.8279(3) 0.0361(3) 0.025(2) Uiso 0.40 1 d PD D 2 F511 F 0.1145(6) 0.8125(4) 0.0415(4) 0.0587(18) Uiso 0.40 1 d PD D 2 F512 F 0.2921(11) 0.7848(7) 0.0540(3) 0.0587(18) Uiso 0.40 1 d PD D 2 F513 F 0.2615(8) 0.8338(5) -0.0075(3) 0.0587(18) Uiso 0.40 1 d PD D 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 0.01395(16) 0.0278(2) 0.02211(19) 0.00079(15) -0.00136(13) 0.00218(14) Mo2 0.01815(17) 0.02207(19) 0.02256(19) 0.00055(15) -0.00154(14) -0.00095(14) Fe1 0.0159(3) 0.0251(3) 0.0197(3) 0.0005(3) -0.0018(2) 0.0017(2) Fe2 0.0184(3) 0.0235(3) 0.0201(3) -0.0007(3) -0.0010(2) -0.0011(2) O1 0.0175(14) 0.037(2) 0.0262(17) 0.0004(15) -0.0011(12) 0.0038(13) O2 0.0230(16) 0.037(2) 0.0261(18) 0.0021(15) -0.0024(13) 0.0048(14) O3 0.0267(16) 0.0298(18) 0.0256(17) 0.0000(14) 0.0009(13) -0.0045(13) O4 0.0266(16) 0.0264(17) 0.0269(18) 0.0029(14) 0.0002(13) -0.0033(13) O5 0.0230(16) 0.0333(19) 0.0328(19) -0.0005(15) -0.0019(14) 0.0025(13) O6 0.0258(16) 0.0290(19) 0.043(2) 0.0032(16) -0.0032(15) 0.0039(14) N1 0.0184(17) 0.028(2) 0.023(2) 0.0006(16) -0.0031(14) 0.0019(14) N2 0.0197(17) 0.027(2) 0.0224(19) -0.0004(16) 0.0022(14) 0.0059(15) N3 0.0238(18) 0.026(2) 0.0215(19) -0.0018(16) 0.0015(15) 0.0030(15) N4 0.0209(17) 0.029(2) 0.0220(19) 0.0000(16) 0.0021(14) 0.0020(15) N5 0.0202(17) 0.025(2) 0.023(2) -0.0016(16) -0.0005(14) -0.0003(14) N6 0.0248(18) 0.025(2) 0.0216(19) 0.0024(16) 0.0015(15) 0.0015(15) N7 0.0247(18) 0.030(2) 0.0200(19) -0.0008(16) -0.0026(15) -0.0002(16) N8 0.0260(19) 0.028(2) 0.0215(19) 0.0007(16) 0.0024(15) -0.0007(16) C1 0.017(2) 0.032(3) 0.029(2) -0.001(2) -0.0044(17) 0.0055(18) C2 0.0134(19) 0.036(3) 0.032(3) 0.003(2) 0.0000(17) 0.0025(17) C3 0.018(2) 0.038(3) 0.030(3) -0.003(2) 0.0027(18) 0.0066(18) C4 0.018(2) 0.030(3) 0.037(3) 0.000(2) -0.0008(18) 0.0057(18) C5 0.019(2) 0.031(3) 0.034(3) 0.004(2) -0.0020(18) 0.0048(18) C6 0.021(2) 0.022(2) 0.031(3) 0.0030(19) -0.0035(18) -0.0008(17) C7 0.023(2) 0.024(2) 0.029(2) 0.0018(19) -0.0012(18) -0.0055(17) C8 0.026(2) 0.022(2) 0.029(2) 0.0009(19) -0.0045(18) -0.0012(18) C9 0.018(2) 0.024(2) 0.031(2) 0.0019(19) -0.0013(17) -0.0011(16) C10 0.021(2) 0.024(2) 0.025(2) 0.0003(18) 0.0000(17) -0.0030(17) C21 0.024(2) 0.043(3) 0.034(3) 0.002(2) -0.005(2) 0.004(2) C22 0.023(2) 0.040(3) 0.039(3) 0.006(2) 0.003(2) 0.002(2) C23 0.027(2) 0.067(4) 0.031(3) -0.003(3) 0.005(2) 0.005(2) C24 0.030(3) 0.039(3) 0.052(4) -0.004(3) -0.003(2) -0.003(2) C25 0.032(3) 0.032(3) 0.040(3) 0.007(2) 0.001(2) 0.003(2) C26 0.021(2) 0.034(3) 0.047(3) 0.003(2) -0.004(2) 0.0019(19) C27 0.036(3) 0.026(3) 0.034(3) -0.004(2) 0.005(2) 0.001(2) C28 0.031(2) 0.032(3) 0.037(3) 0.002(2) -0.011(2) -0.004(2) C29 0.023(2) 0.034(3) 0.043(3) 0.005(2) 0.000(2) 0.003(2) C30 0.033(3) 0.035(3) 0.031(3) 0.001(2) -0.001(2) 0.001(2) C41 0.019(2) 0.031(2) 0.027(2) 0.000(2) -0.0002(17) 0.0050(17) C42 0.027(2) 0.033(3) 0.023(2) 0.001(2) -0.0051(18) 0.0066(19) C43 0.022(2) 0.032(3) 0.026(2) -0.004(2) -0.0029(18) 0.0025(18) C44 0.027(2) 0.027(2) 0.030(3) 0.002(2) 0.0014(19) -0.0044(18) C45 0.030(2) 0.031(3) 0.021(2) -0.0033(19) 0.0002(18) -0.0013(19) C46 0.020(2) 0.032(3) 0.036(3) 0.004(2) -0.0067(19) -0.0033(18) C53 0.021(2) 0.027(2) 0.026(2) -0.0005(19) 0.0016(17) 0.0037(17) C54 0.031(2) 0.026(2) 0.021(2) -0.0012(19) -0.0002(18) 0.0027(18) C55 0.026(2) 0.026(2) 0.022(2) 0.0004(19) -0.0033(18) -0.0007(18) C56 0.029(2) 0.025(2) 0.024(2) 0.0044(19) 0.0022(18) -0.0023(18) C57 0.022(2) 0.031(3) 0.027(2) -0.002(2) -0.0022(18) 0.0006(18) C58 0.028(2) 0.027(2) 0.023(2) 0.0009(19) 0.0014(18) -0.0001(18) C65 0.028(2) 0.035(3) 0.034(3) -0.002(2) -0.004(2) 0.009(2) C66 0.038(3) 0.031(3) 0.044(3) -0.002(2) -0.001(2) 0.009(2) C67 0.030(2) 0.030(3) 0.038(3) -0.003(2) 0.001(2) 0.001(2) C68 0.022(2) 0.030(2) 0.028(2) -0.003(2) -0.0005(18) 0.0038(18) C69 0.051(3) 0.035(3) 0.030(3) 0.002(2) -0.010(2) 0.000(2) C70 0.058(4) 0.033(3) 0.036(3) 0.010(2) -0.005(3) -0.009(3) C71 0.043(3) 0.039(3) 0.044(3) 0.000(3) 0.003(3) -0.011(2) C72 0.027(2) 0.032(3) 0.032(3) 0.001(2) 0.0012(19) -0.0004(19) C73 0.036(3) 0.030(3) 0.028(3) -0.003(2) -0.006(2) 0.001(2) C74 0.043(3) 0.031(3) 0.032(3) -0.005(2) 0.000(2) -0.002(2) C75 0.034(3) 0.030(3) 0.035(3) -0.001(2) 0.006(2) 0.008(2) C76 0.025(2) 0.033(3) 0.028(3) 0.002(2) 0.0021(18) 0.0053(19) C77 0.026(2) 0.029(3) 0.028(2) 0.002(2) -0.0041(18) 0.0013(19) C78 0.031(2) 0.038(3) 0.037(3) -0.001(2) -0.004(2) 0.012(2) C79 0.045(3) 0.029(3) 0.040(3) 0.000(2) -0.006(2) 0.013(2) C80 0.038(3) 0.025(2) 0.033(3) 0.000(2) -0.001(2) 0.002(2) C81 0.031(2) 0.029(3) 0.027(2) 0.002(2) -0.0013(19) -0.0008(19) C82 0.043(3) 0.033(3) 0.029(3) 0.002(2) -0.001(2) 0.009(2) C83 0.044(3) 0.039(3) 0.027(3) 0.001(2) -0.009(2) 0.010(2) C84 0.035(3) 0.036(3) 0.034(3) -0.005(2) -0.012(2) 0.001(2) C85 0.042(3) 0.029(3) 0.030(3) 0.001(2) 0.006(2) 0.001(2) C86 0.034(3) 0.038(3) 0.033(3) 0.003(2) 0.012(2) 0.008(2) C87 0.029(2) 0.035(3) 0.033(3) 0.004(2) 0.006(2) 0.003(2) C88 0.024(2) 0.032(3) 0.025(2) 0.002(2) 0.0027(18) 0.0009(18) Mo3 0.02041(18) 0.0277(2) 0.0290(2) 0.00794(17) -0.00403(15) -0.00347(15) Mo4 0.01704(16) 0.0285(2) 0.0246(2) 0.00348(16) -0.00146(14) -0.00389(14) Fe3 0.0185(3) 0.0258(3) 0.0237(3) 0.0042(3) -0.0008(2) -0.0010(2) Fe4 0.0262(3) 0.0292(4) 0.0263(4) 0.0070(3) -0.0071(3) -0.0061(3) N9 0.0242(18) 0.028(2) 0.025(2) 0.0032(17) -0.0002(15) 0.0016(15) N10 0.0245(19) 0.026(2) 0.027(2) 0.0016(17) -0.0012(15) -0.0004(15) N11 0.0232(18) 0.031(2) 0.0213(19) 0.0048(16) -0.0045(15) 0.0008(15) N12 0.0225(18) 0.028(2) 0.025(2) 0.0057(16) -0.0049(15) -0.0059(15) N13 0.027(2) 0.031(2) 0.031(2) 0.0082(18) -0.0066(17) -0.0022(16) N14 0.035(2) 0.036(2) 0.028(2) 0.0139(19) -0.0086(18) -0.0102(18) N15 0.0248(19) 0.032(2) 0.025(2) 0.0047(17) -0.0042(16) -0.0035(16) N16 0.033(2) 0.035(2) 0.029(2) 0.0104(19) -0.0063(17) -0.0081(18) O7 0.0277(16) 0.0284(18) 0.0313(19) 0.0046(15) -0.0027(14) 0.0006(13) O8 0.0346(18) 0.034(2) 0.0315(19) 0.0082(16) -0.0094(15) -0.0039(15) O9 0.0243(16) 0.042(2) 0.0292(19) 0.0062(16) -0.0065(14) -0.0075(14) O10 0.0188(15) 0.0363(19) 0.0323(19) 0.0034(15) -0.0026(13) -0.0002(13) O11 0.0270(17) 0.037(2) 0.046(2) 0.0092(18) -0.0054(16) -0.0055(15) O12 0.0242(16) 0.036(2) 0.035(2) 0.0028(16) 0.0016(14) -0.0051(14) C11 0.029(2) 0.028(3) 0.040(3) 0.010(2) -0.001(2) 0.0022(19) C12 0.026(2) 0.023(2) 0.037(3) 0.005(2) -0.004(2) -0.0031(18) C13 0.022(2) 0.024(2) 0.038(3) 0.010(2) -0.0045(19) -0.0012(17) C14 0.021(2) 0.033(3) 0.033(3) 0.013(2) -0.0028(19) -0.0043(18) C15 0.019(2) 0.036(3) 0.042(3) 0.015(2) -0.004(2) 0.0006(19) C16 0.016(2) 0.035(3) 0.037(3) 0.003(2) 0.0013(18) -0.0063(18) C17 0.018(2) 0.033(3) 0.034(3) 0.005(2) -0.0016(18) -0.0044(18) C18 0.020(2) 0.031(3) 0.037(3) 0.002(2) -0.0037(19) -0.0056(18) C19 0.019(2) 0.029(3) 0.036(3) 0.002(2) -0.0022(18) -0.0047(18) C20 0.020(2) 0.032(3) 0.033(3) 0.004(2) -0.0002(18) -0.0062(18) C31 0.044(3) 0.039(3) 0.041(3) 0.005(3) 0.008(2) 0.009(2) C32 0.034(3) 0.032(3) 0.041(3) 0.003(2) -0.009(2) -0.002(2) C33 0.023(2) 0.036(3) 0.041(3) 0.007(2) -0.001(2) -0.002(2) C34 0.031(3) 0.049(3) 0.039(3) 0.015(3) -0.009(2) -0.005(2) C35 0.021(2) 0.055(4) 0.058(4) 0.019(3) -0.001(2) 0.000(2) C36 0.030(3) 0.047(3) 0.039(3) 0.000(3) 0.001(2) 0.002(2) C37 0.024(2) 0.039(3) 0.044(3) 0.004(2) -0.002(2) 0.001(2) C38 0.033(3) 0.041(3) 0.035(3) 0.001(2) -0.011(2) 0.001(2) C39 0.036(3) 0.035(3) 0.041(3) -0.001(2) -0.005(2) 0.003(2) C40 0.025(2) 0.042(3) 0.039(3) 0.011(2) -0.001(2) -0.005(2) C47 0.024(2) 0.031(3) 0.030(3) 0.004(2) 0.0031(19) 0.0031(19) C48 0.029(2) 0.032(3) 0.027(2) 0.007(2) 0.0042(19) -0.0010(19) C49 0.0167(19) 0.033(3) 0.030(2) 0.005(2) 0.0008(17) -0.0026(17) C50 0.036(3) 0.030(3) 0.038(3) 0.011(2) -0.012(2) -0.002(2) C51 0.030(2) 0.036(3) 0.030(3) 0.003(2) -0.008(2) 0.001(2) C52 0.028(2) 0.038(3) 0.047(3) 0.013(3) -0.006(2) -0.001(2) C59 0.033(2) 0.028(3) 0.029(3) 0.007(2) -0.003(2) 0.000(2) C60 0.026(2) 0.032(3) 0.023(2) 0.004(2) -0.0034(18) -0.0037(19) C61 0.021(2) 0.032(3) 0.029(3) 0.008(2) -0.0007(18) -0.0035(18) C62 0.037(3) 0.034(3) 0.032(3) 0.009(2) -0.013(2) -0.006(2) C63 0.033(2) 0.025(2) 0.029(3) 0.005(2) -0.008(2) -0.0026(19) C64 0.026(2) 0.040(3) 0.034(3) 0.009(2) -0.005(2) -0.005(2) C89 0.040(3) 0.036(3) 0.030(3) 0.003(2) 0.005(2) 0.002(2) C90 0.048(3) 0.034(3) 0.032(3) -0.005(2) 0.002(2) -0.001(2) C91 0.035(3) 0.035(3) 0.038(3) -0.002(2) -0.004(2) -0.003(2) C92 0.029(2) 0.031(3) 0.028(3) 0.001(2) -0.0002(19) -0.0009(19) C93 0.042(3) 0.035(3) 0.030(3) 0.008(2) 0.001(2) -0.002(2) C94 0.048(3) 0.037(3) 0.029(3) 0.006(2) -0.004(2) 0.008(2) C95 0.044(3) 0.034(3) 0.037(3) 0.003(2) -0.007(2) 0.011(2) C96 0.026(2) 0.037(3) 0.030(3) 0.000(2) -0.0070(19) 0.007(2) C97 0.023(2) 0.038(3) 0.034(3) 0.003(2) 0.0011(19) -0.005(2) C98 0.030(2) 0.031(3) 0.048(3) 0.003(2) 0.000(2) -0.007(2) C99 0.027(2) 0.030(3) 0.038(3) 0.002(2) -0.002(2) 0.0030(19) C100 0.020(2) 0.034(3) 0.027(2) 0.002(2) -0.0014(17) -0.0009(18) C101 0.052(3) 0.037(3) 0.047(4) 0.019(3) -0.014(3) -0.011(3) C102 0.052(4) 0.041(4) 0.052(4) 0.015(3) -0.012(3) -0.019(3) C103 0.037(3) 0.059(4) 0.048(4) 0.019(3) -0.012(3) -0.023(3) C104 0.034(3) 0.046(3) 0.034(3) 0.016(2) -0.005(2) -0.012(2) C105 0.037(3) 0.028(3) 0.042(3) 0.005(2) -0.013(2) -0.001(2) C106 0.038(3) 0.030(3) 0.046(3) 0.007(2) -0.017(2) -0.008(2) C107 0.029(2) 0.038(3) 0.037(3) 0.006(2) -0.009(2) -0.001(2) C108 0.031(2) 0.032(3) 0.034(3) 0.003(2) -0.006(2) -0.001(2) C109 0.029(3) 0.053(4) 0.044(3) 0.013(3) -0.003(2) -0.004(2) C110 0.033(3) 0.056(4) 0.044(3) 0.020(3) -0.005(2) -0.011(3) C111 0.040(3) 0.047(3) 0.040(3) 0.021(3) -0.012(2) -0.014(3) C112 0.039(3) 0.031(3) 0.035(3) 0.009(2) -0.009(2) -0.010(2) O201 0.087(4) 0.065(4) 0.071(4) -0.026(3) 0.030(3) 0.005(3) O202 0.039(2) 0.048(3) 0.068(3) -0.005(2) -0.012(2) -0.0003(19) O203 0.048(2) 0.043(2) 0.048(3) 0.008(2) -0.0014(19) 0.0005(19) S200 0.0351(7) 0.0376(7) 0.0445(8) -0.0073(6) -0.0005(6) 0.0021(5) C200 0.043(3) 0.060(4) 0.033(3) 0.011(3) 0.002(2) -0.009(3) F201 0.058(2) 0.070(3) 0.069(3) 0.010(2) 0.012(2) 0.030(2) F202 0.054(2) 0.096(4) 0.057(3) 0.019(2) -0.022(2) -0.014(2) F203 0.059(2) 0.077(3) 0.070(3) 0.035(2) 0.004(2) -0.007(2) O301 0.0370(19) 0.046(2) 0.032(2) 0.0112(17) -0.0014(16) 0.0072(17) O302 0.0362(19) 0.036(2) 0.042(2) -0.0061(17) 0.0040(17) -0.0055(16) O303 0.0332(18) 0.036(2) 0.0298(19) 0.0077(16) 0.0032(15) -0.0036(15) S300 0.0280(5) 0.0269(6) 0.0267(6) 0.0011(5) 0.0001(4) 0.0013(4) C300 0.030(2) 0.038(3) 0.038(3) -0.002(2) -0.006(2) 0.003(2) F301 0.0435(19) 0.052(2) 0.057(2) -0.0083(18) 0.0214(17) -0.0008(16) F302 0.051(2) 0.065(3) 0.069(3) -0.006(2) -0.0191(19) 0.0332(19) F303 0.0440(18) 0.0364(18) 0.055(2) -0.0131(16) 0.0015(16) -0.0015(14) N600 0.043(3) 0.045(3) 0.032(2) 0.001(2) 0.002(2) 0.009(2) C601 0.040(3) 0.033(3) 0.032(3) 0.004(2) 0.000(2) 0.001(2) C602 0.037(3) 0.041(3) 0.055(4) 0.007(3) 0.015(3) 0.005(2) N700 0.037(3) 0.049(3) 0.060(4) 0.011(3) 0.007(2) 0.008(2) C701 0.027(2) 0.048(4) 0.037(3) 0.006(3) -0.002(2) 0.007(2) C702 0.069(4) 0.038(3) 0.048(4) 0.003(3) -0.022(3) 0.005(3) N800 0.047(3) 0.055(4) 0.047(3) 0.004(3) 0.001(2) -0.008(3) C801 0.028(2) 0.050(4) 0.037(3) 0.004(3) 0.002(2) 0.003(2) C802 0.050(4) 0.049(4) 0.070(5) -0.003(4) 0.002(3) -0.003(3) N900 0.050(2) 0.054(2) 0.042(2) 0.004(2) -0.0068(19) 0.000(2) C901 0.045(4) 0.048(4) 0.042(4) 0.005(3) -0.003(3) 0.007(3) C902 0.065(5) 0.070(5) 0.071(5) 0.007(3) -0.005(3) 0.005(3) C911 0.041(6) 0.040(6) 0.039(6) 0.002(3) -0.001(3) 0.005(3) C912 0.060(8) 0.062(8) 0.060(8) 0.004(3) 0.000(3) 0.005(3) O401 0.082(3) 0.080(3) 0.071(2) -0.006(2) 0.0228(19) -0.0003(19) O402 0.082(3) 0.084(4) 0.096(3) 0.002(3) -0.027(2) 0.006(3) O403 0.045(2) 0.049(3) 0.044(3) 0.006(2) 0.013(2) 0.002(2) S400 0.0514(15) 0.0314(14) 0.0513(17) -0.0112(12) 0.0042(12) -0.0035(11) C400 0.052(2) 0.046(2) 0.061(3) 0.015(2) 0.011(2) 0.001(2) F401 0.045(2) 0.046(2) 0.047(2) -0.0002(19) 0.0058(18) -0.0065(17) F402 0.083(3) 0.103(4) 0.116(4) 0.017(3) -0.021(3) 0.010(3) F403 0.090(3) 0.083(3) 0.083(3) -0.002(2) 0.024(2) 0.014(2) O411 0.082(3) 0.080(3) 0.071(2) -0.006(2) 0.0228(19) -0.0003(19) O412 0.045(5) 0.042(5) 0.038(5) 0.008(3) 0.006(3) 0.003(3) O413 0.055(5) 0.054(5) 0.057(5) -0.003(3) 0.004(3) 0.007(3) S410 0.041(3) 0.026(2) 0.035(3) 0.0001(18) 0.0078(19) -0.0003(18) C410 0.035(4) 0.033(5) 0.038(5) 0.000(3) -0.002(3) 0.004(3) F411 0.059(4) 0.061(4) 0.057(4) 0.004(3) -0.001(3) 0.000(3) F412 0.060(4) 0.061(4) 0.064(4) -0.001(3) -0.004(3) 0.007(3) F413 0.040(4) 0.047(4) 0.045(4) 0.001(3) -0.001(3) 0.003(3) S500 0.0362(10) 0.0295(10) 0.0402(12) -0.0059(9) -0.0130(9) 0.0046(8) O501 0.056(3) 0.052(3) 0.048(3) -0.004(2) -0.027(2) 0.012(2) O502 0.087(3) 0.080(4) 0.079(3) 0.001(3) 0.030(2) 0.016(3) O503 0.041(3) 0.041(3) 0.040(3) 0.007(2) -0.007(2) 0.0096(19) C500 0.049(3) 0.045(2) 0.061(3) 0.018(2) -0.015(2) 0.0046(16) F501 0.103(4) 0.109(4) 0.103(3) 0.008(3) 0.024(3) 0.016(3) F502 0.039(2) 0.041(2) 0.043(3) 0.011(2) -0.003(2) 0.0080(18) F503 0.088(3) 0.076(3) 0.085(3) 0.006(3) -0.040(3) 0.000(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 O5 1.729(4) . ? Mo1 O2 1.749(4) . ? Mo1 O1 1.798(3) . ? Mo1 C1 2.398(5) . ? Mo1 C5 2.412(5) . ? Mo1 C2 2.442(5) . ? Mo1 C4 2.445(5) . ? Mo1 C3 2.480(5) . ? Mo2 O6 1.731(4) . ? Mo2 O4 1.756(4) . ? Mo2 O3 1.788(4) . ? Mo2 C8 2.396(5) . ? Mo2 C9 2.431(5) . ? Mo2 C7 2.443(5) . ? Mo2 C6 2.455(5) . ? Mo2 C10 2.460(5) . ? Fe1 O1 1.962(3) . ? Fe1 O4 2.153(4) . ? Fe1 N4 2.186(4) . ? Fe1 N3 2.198(4) . ? Fe1 N2 2.207(4) . ? Fe1 N1 2.240(4) . ? Fe2 O3 1.967(4) . ? Fe2 O2 2.120(4) . ? Fe2 N8 2.187(4) . ? Fe2 N7 2.214(4) . ? Fe2 N5 2.231(4) . ? Fe2 N6 2.261(4) . ? N1 C43 1.469(7) . ? N1 C41 1.477(7) . ? N1 C42 1.488(6) . ? N2 C68 1.342(7) . ? N2 C53 1.346(6) . ? N3 C54 1.344(6) . ? N3 C72 1.343(6) . ? N4 C76 1.343(7) . ? N4 C55 1.343(6) . ? N5 C46 1.472(6) . ? N5 C44 1.474(7) . ? N5 C45 1.484(7) . ? N6 C77 1.328(6) . ? N6 C56 1.348(7) . ? N7 C81 1.338(7) . ? N7 C57 1.350(6) . ? N8 C58 1.339(7) . ? N8 C88 1.346(6) . ? C1 C2 1.427(7) . ? C1 C5 1.431(7) . ? C1 C21 1.488(8) . ? C2 C3 1.418(8) . ? C2 C22 1.478(7) . ? C3 C4 1.420(8) . ? C3 C23 1.487(8) . ? C4 C5 1.415(8) . ? C4 C24 1.508(8) . ? C5 C25 1.498(8) . ? C6 C10 1.424(7) . ? C6 C7 1.425(7) . ? C6 C26 1.502(7) . ? C7 C8 1.428(7) . ? C7 C27 1.490(8) . ? C8 C9 1.416(8) . ? C8 C28 1.506(7) . ? C9 C10 1.411(7) . ? C9 C29 1.499(7) . ? C10 C30 1.510(7) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C41 C53 1.504(7) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C54 1.506(7) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C55 1.512(7) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C56 1.511(7) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C58 1.509(7) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C57 1.499(7) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C53 C65 1.379(8) . ? C54 C69 1.383(8) . ? C55 C73 1.378(8) . ? C56 C80 1.384(8) . ? C57 C84 1.376(7) . ? C58 C85 1.382(8) . ? C65 C66 1.377(8) . ? C65 H65 0.9500 . ? C66 C67 1.381(8) . ? C66 H66 0.9500 . ? C67 C68 1.371(8) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C70 1.384(9) . ? C69 H69 0.9500 . ? C70 C71 1.383(9) . ? C70 H70 0.9500 . ? C71 C72 1.372(8) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C74 1.381(9) . ? C73 H73 0.9500 . ? C74 C75 1.379(8) . ? C74 H74 0.9500 . ? C75 C76 1.391(8) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C77 C78 1.395(8) . ? C77 H77 0.9500 . ? C78 C79 1.371(9) . ? C78 H78 0.9500 . ? C79 C80 1.390(8) . ? C79 H79 0.9500 . ? C80 H80 0.9500 . ? C81 C82 1.379(8) . ? C81 H81 0.9500 . ? C82 C83 1.371(8) . ? C82 H82 0.9500 . ? C83 C84 1.384(9) . ? C83 H83 0.9500 . ? C84 H84 0.9500 . ? C85 C86 1.382(8) . ? C85 H85 0.9500 . ? C86 C87 1.388(9) . ? C86 H86 0.9500 . ? C87 C88 1.372(8) . ? C87 H87 0.9500 . ? C88 H88 0.9500 . ? Mo3 O11 1.728(4) . ? Mo3 O7 1.757(4) . ? Mo3 O8 1.788(4) . ? Mo3 C11 2.410(6) . ? Mo3 C14 2.437(5) . ? Mo3 C15 2.441(5) . ? Mo3 C13 2.441(5) . ? Mo3 C12 2.449(5) . ? Mo4 O12 1.725(4) . ? Mo4 O9 1.756(4) . ? Mo4 O10 1.788(4) . ? Mo4 C16 2.393(5) . ? Mo4 C20 2.416(5) . ? Mo4 C17 2.441(5) . ? Mo4 C19 2.443(5) . ? Mo4 C18 2.479(5) . ? Fe3 O10 1.968(4) . ? Fe3 O7 2.121(4) . ? Fe3 N10 2.189(5) . ? Fe3 N11 2.211(4) . ? Fe3 N12 2.213(4) . ? Fe3 N9 2.240(4) . ? Fe4 O8 1.968(5) . ? Fe4 O9 2.138(4) . ? Fe4 N15 2.205(4) . ? Fe4 N16 2.213(5) . ? Fe4 N13 2.229(5) . ? Fe4 N14 2.235(4) . ? N9 C47 1.461(7) . ? N9 C49 1.482(6) . ? N9 C48 1.489(7) . ? N10 C92 1.348(7) . ? N10 C59 1.351(7) . ? N11 C60 1.339(7) . ? N11 C96 1.345(7) . ? N12 C100 1.325(7) . ? N12 C61 1.360(6) . ? N13 C50 1.473(7) . ? N13 C52 1.477(7) . ? N13 C51 1.491(7) . ? N14 C62 1.343(8) . ? N14 C104 1.345(8) . ? N15 C63 1.329(8) . ? N15 C108 1.343(7) . ? N16 C112 1.339(7) . ? N16 C64 1.345(8) . ? C11 C12 1.430(7) . ? C11 C15 1.428(8) . ? C11 C31 1.498(9) . ? C12 C13 1.416(8) . ? C12 C32 1.506(7) . ? C13 C14 1.431(7) . ? C13 C33 1.484(7) . ? C14 C15 1.403(8) . ? C14 C34 1.501(8) . ? C15 C35 1.502(7) . ? C16 C20 1.418(8) . ? C16 C17 1.428(8) . ? C16 C36 1.498(9) . ? C17 C18 1.401(8) . ? C17 C37 1.506(8) . ? C18 C19 1.441(8) . ? C18 C38 1.487(8) . ? C19 C20 1.427(8) . ? C19 C39 1.499(8) . ? C20 C40 1.499(8) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C47 C59 1.516(7) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C60 1.501(8) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C61 1.504(8) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C62 1.493(9) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C63 1.515(8) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C64 1.501(8) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C59 C89 1.382(9) . ? C60 C93 1.389(8) . ? C61 C97 1.380(8) . ? C62 C101 1.391(8) . ? C63 C105 1.391(7) . ? C64 C109 1.381(8) . ? C89 C90 1.392(8) . ? C89 H89 0.9500 . ? C90 C91 1.379(9) . ? C90 H90 0.9500 . ? C91 C92 1.375(8) . ? C91 H91 0.9500 . ? C92 H92 0.9500 . ? C93 C94 1.375(9) . ? C93 H93 0.9500 . ? C94 C95 1.386(9) . ? C94 H94 0.9500 . ? C95 C96 1.376(8) . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? C97 C98 1.369(9) . ? C97 H97 0.9500 . ? C98 C99 1.381(8) . ? C98 H98 0.9500 . ? C99 C100 1.382(8) . ? C99 H99 0.9500 . ? C100 H100 0.9500 . ? C101 C102 1.385(10) . ? C101 H101 0.9500 . ? C102 C103 1.372(11) . ? C102 H102 0.9500 . ? C103 C104 1.390(8) . ? C103 H103 0.9500 . ? C104 H104 0.9500 . ? C105 C106 1.379(9) . ? C105 H105 0.9500 . ? C106 C107 1.391(9) . ? C106 H106 0.9500 . ? C107 C108 1.390(7) . ? C107 H107 0.9500 . ? C108 H108 0.9500 . ? C109 C110 1.391(10) . ? C109 H109 0.9500 . ? C110 C111 1.369(11) . ? C110 H110 0.9500 . ? C111 C112 1.392(8) . ? C111 H111 0.9500 . ? C112 H112 0.9500 . ? O201 S200 1.423(6) . ? O202 S200 1.426(5) . ? O203 S200 1.443(5) . ? S200 C200 1.815(8) . ? C200 F201 1.321(9) . ? C200 F202 1.336(8) . ? C200 F203 1.344(7) . ? O301 S300 1.433(4) . ? O302 S300 1.437(4) . ? O303 S300 1.445(4) . ? S300 C300 1.822(6) . ? C300 F302 1.327(7) . ? C300 F303 1.330(7) . ? C300 F301 1.338(7) . ? N600 C601 1.140(8) . ? C601 C602 1.452(9) . ? C602 H60A 0.9800 . ? C602 H60B 0.9800 . ? C602 H60C 0.9800 . ? N700 C701 1.135(8) . ? C701 C702 1.461(9) . ? C702 H70A 0.9800 . ? C702 H70B 0.9800 . ? C702 H70C 0.9800 . ? N800 C801 1.137(9) . ? C801 C802 1.441(10) . ? C802 H80A 0.9800 . ? C802 H80B 0.9800 . ? C802 H80C 0.9800 . ? N900 C901 1.076(13) . ? C901 C902 1.468(17) . ? C902 H90A 0.9800 . ? C902 H90B 0.9800 . ? C902 H90C 0.9800 . ? C911 C912 1.49(3) . ? C912 H91A 0.9800 . ? C912 H91B 0.9800 . ? C912 H91C 0.9800 . ? O401 S400 1.436(2) . ? O402 S400 1.431(2) . ? O403 S400 1.440(2) . ? S400 C400 1.816(2) . ? C400 F402 1.331(2) . ? C400 F401 1.332(2) . ? C400 F403 1.336(2) . ? O411 S410 1.434(2) . ? O412 S410 1.435(2) . ? O412 C410 1.957(19) . ? O413 S410 1.433(2) . ? S410 C410 1.818(2) . ? C410 F412 1.334(2) . ? C410 F411 1.334(2) . ? C410 F413 1.335(2) . ? S500 O501 1.433(2) . ? S500 O503 1.433(2) . ? S500 O502 1.434(2) . ? S500 C500 1.816(2) . ? C500 F502 1.334(2) . ? C500 F503 1.334(2) . ? C500 F501 1.336(2) . ? S510 O512 1.434(2) . ? S510 O511 1.434(2) . ? S510 O513 1.438(2) . ? S510 C510 1.818(2) . ? C510 F512 1.335(2) . ? C510 F513 1.335(2) . ? C510 F511 1.336(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Mo1 O2 104.53(18) . . ? O5 Mo1 O1 106.02(17) . . ? O2 Mo1 O1 107.33(16) . . ? O5 Mo1 C1 92.54(17) . . ? O2 Mo1 C1 102.86(17) . . ? O1 Mo1 C1 138.80(18) . . ? O5 Mo1 C5 126.46(17) . . ? O2 Mo1 C5 86.54(18) . . ? O1 Mo1 C5 120.46(18) . . ? C1 Mo1 C5 34.61(17) . . ? O5 Mo1 C2 84.29(18) . . ? O2 Mo1 C2 137.12(17) . . ? O1 Mo1 C2 110.25(17) . . ? C1 Mo1 C2 34.28(18) . . ? C5 Mo1 C2 56.83(17) . . ? O5 Mo1 C4 140.22(17) . . ? O2 Mo1 C4 106.35(18) . . ? O1 Mo1 C4 88.02(17) . . ? C1 Mo1 C4 56.56(17) . . ? C5 Mo1 C4 33.87(19) . . ? C2 Mo1 C4 55.98(17) . . ? O5 Mo1 C3 110.23(18) . . ? O2 Mo1 C3 139.48(18) . . ? O1 Mo1 C3 82.66(17) . . ? C1 Mo1 C3 56.27(18) . . ? C5 Mo1 C3 56.17(18) . . ? C2 Mo1 C3 33.47(18) . . ? C4 Mo1 C3 33.50(18) . . ? O6 Mo2 O4 104.91(18) . . ? O6 Mo2 O3 105.77(19) . . ? O4 Mo2 O3 107.60(16) . . ? O6 Mo2 C8 91.41(18) . . ? O4 Mo2 C8 103.30(18) . . ? O3 Mo2 C8 138.93(17) . . ? O6 Mo2 C9 84.88(17) . . ? O4 Mo2 C9 137.27(18) . . ? O3 Mo2 C9 109.39(17) . . ? C8 Mo2 C9 34.11(18) . . ? O6 Mo2 C7 124.65(17) . . ? O4 Mo2 C7 85.59(17) . . ? O3 Mo2 C7 122.73(17) . . ? C8 Mo2 C7 34.32(17) . . ? C9 Mo2 C7 56.52(17) . . ? O6 Mo2 C6 140.85(17) . . ? O4 Mo2 C6 103.99(18) . . ? O3 Mo2 C6 89.87(17) . . ? C8 Mo2 C6 56.41(16) . . ? C9 Mo2 C6 55.99(16) . . ? C7 Mo2 C6 33.81(17) . . ? O6 Mo2 C10 111.78(17) . . ? O4 Mo2 C10 137.49(17) . . ? O3 Mo2 C10 82.67(16) . . ? C8 Mo2 C10 56.27(17) . . ? C9 Mo2 C10 33.54(16) . . ? C7 Mo2 C10 56.20(17) . . ? C6 Mo2 C10 33.68(17) . . ? O1 Fe1 O4 94.20(14) . . ? O1 Fe1 N4 111.97(16) . . ? O4 Fe1 N4 87.64(15) . . ? O1 Fe1 N3 95.04(15) . . ? O4 Fe1 N3 170.55(14) . . ? N4 Fe1 N3 90.79(16) . . ? O1 Fe1 N2 96.74(15) . . ? O4 Fe1 N2 96.79(15) . . ? N4 Fe1 N2 150.60(15) . . ? N3 Fe1 N2 80.12(16) . . ? O1 Fe1 N1 170.89(16) . . ? O4 Fe1 N1 92.40(14) . . ? N4 Fe1 N1 74.56(16) . . ? N3 Fe1 N1 78.21(15) . . ? N2 Fe1 N1 76.22(15) . . ? O3 Fe2 O2 93.19(15) . . ? O3 Fe2 N8 94.94(16) . . ? O2 Fe2 N8 170.38(16) . . ? O3 Fe2 N7 110.98(16) . . ? O2 Fe2 N7 89.30(15) . . ? N8 Fe2 N7 92.56(16) . . ? O3 Fe2 N5 171.97(16) . . ? O2 Fe2 N5 92.86(15) . . ? N8 Fe2 N5 78.59(16) . . ? N7 Fe2 N5 74.36(16) . . ? O3 Fe2 N6 98.83(16) . . ? O2 Fe2 N6 95.58(15) . . ? N8 Fe2 N6 78.12(16) . . ? N7 Fe2 N6 149.48(16) . . ? N5 Fe2 N6 75.32(15) . . ? Mo1 O1 Fe1 150.7(2) . . ? Mo1 O2 Fe2 164.3(2) . . ? Mo2 O3 Fe2 150.0(2) . . ? Mo2 O4 Fe1 155.8(2) . . ? C43 N1 C41 112.3(4) . . ? C43 N1 C42 110.9(4) . . ? C41 N1 C42 111.8(4) . . ? C43 N1 Fe1 106.0(3) . . ? C41 N1 Fe1 105.8(3) . . ? C42 N1 Fe1 109.7(3) . . ? C68 N2 C53 117.7(4) . . ? C68 N2 Fe1 124.1(3) . . ? C53 N2 Fe1 114.2(3) . . ? C54 N3 C72 117.7(5) . . ? C54 N3 Fe1 114.7(3) . . ? C72 N3 Fe1 125.4(4) . . ? C76 N4 C55 118.6(5) . . ? C76 N4 Fe1 125.9(3) . . ? C55 N4 Fe1 115.5(3) . . ? C46 N5 C44 111.6(4) . . ? C46 N5 C45 110.2(4) . . ? C44 N5 C45 111.9(4) . . ? C46 N5 Fe2 106.6(3) . . ? C44 N5 Fe2 107.3(3) . . ? C45 N5 Fe2 109.0(3) . . ? C77 N6 C56 118.2(5) . . ? C77 N6 Fe2 123.9(3) . . ? C56 N6 Fe2 113.6(3) . . ? C81 N7 C57 117.7(4) . . ? C81 N7 Fe2 127.2(3) . . ? C57 N7 Fe2 115.0(3) . . ? C58 N8 C88 118.0(5) . . ? C58 N8 Fe2 114.3(3) . . ? C88 N8 Fe2 125.2(4) . . ? C2 C1 C5 107.9(5) . . ? C2 C1 C21 124.2(5) . . ? C5 C1 C21 127.7(5) . . ? C2 C1 Mo1 74.6(3) . . ? C5 C1 Mo1 73.2(3) . . ? C21 C1 Mo1 122.8(4) . . ? C3 C2 C1 108.0(5) . . ? C3 C2 C22 127.5(5) . . ? C1 C2 C22 124.5(5) . . ? C3 C2 Mo1 74.8(3) . . ? C1 C2 Mo1 71.2(3) . . ? C22 C2 Mo1 120.2(4) . . ? C2 C3 C4 107.9(5) . . ? C2 C3 C23 127.1(5) . . ? C4 C3 C23 125.0(5) . . ? C2 C3 Mo1 71.8(3) . . ? C4 C3 Mo1 71.9(3) . . ? C23 C3 Mo1 121.3(4) . . ? C5 C4 C3 108.7(5) . . ? C5 C4 C24 125.6(5) . . ? C3 C4 C24 125.6(5) . . ? C5 C4 Mo1 71.8(3) . . ? C3 C4 Mo1 74.6(3) . . ? C24 C4 Mo1 121.4(4) . . ? C4 C5 C1 107.5(5) . . ? C4 C5 C25 125.6(5) . . ? C1 C5 C25 126.9(5) . . ? C4 C5 Mo1 74.4(3) . . ? C1 C5 Mo1 72.1(3) . . ? C25 C5 Mo1 121.5(4) . . ? C10 C6 C7 108.3(4) . . ? C10 C6 C26 125.0(5) . . ? C7 C6 C26 126.7(5) . . ? C10 C6 Mo2 73.3(3) . . ? C7 C6 Mo2 72.6(3) . . ? C26 C6 Mo2 120.7(3) . . ? C6 C7 C8 107.0(5) . . ? C6 C7 C27 125.7(5) . . ? C8 C7 C27 127.3(5) . . ? C6 C7 Mo2 73.6(3) . . ? C8 C7 Mo2 71.0(3) . . ? C27 C7 Mo2 121.6(3) . . ? C9 C8 C7 108.4(4) . . ? C9 C8 C28 124.0(5) . . ? C7 C8 C28 127.3(5) . . ? C9 C8 Mo2 74.3(3) . . ? C7 C8 Mo2 74.6(3) . . ? C28 C8 Mo2 121.0(3) . . ? C10 C9 C8 108.2(4) . . ? C10 C9 C29 127.6(5) . . ? C8 C9 C29 124.2(5) . . ? C10 C9 Mo2 74.4(3) . . ? C8 C9 Mo2 71.6(3) . . ? C29 C9 Mo2 119.2(4) . . ? C9 C10 C6 108.0(4) . . ? C9 C10 C30 127.5(5) . . ? C6 C10 C30 124.5(4) . . ? C9 C10 Mo2 72.1(3) . . ? C6 C10 Mo2 73.0(3) . . ? C30 C10 Mo2 121.7(3) . . ? C1 C21 H21A 109.5 . . ? C1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C2 C22 H22A 109.5 . . ? C2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C3 C23 H23A 109.5 . . ? C3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C4 C24 H24A 109.5 . . ? C4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C5 C25 H25A 109.5 . . ? C5 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C5 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C6 C26 H26A 109.5 . . ? C6 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C6 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C7 C27 H27A 109.5 . . ? C7 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C7 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C8 C28 H28A 109.5 . . ? C8 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C8 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C9 C29 H29A 109.5 . . ? C9 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C9 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C10 C30 H30A 109.5 . . ? C10 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C10 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N1 C41 C53 108.8(4) . . ? N1 C41 H41A 109.9 . . ? C53 C41 H41A 109.9 . . ? N1 C41 H41B 109.9 . . ? C53 C41 H41B 109.9 . . ? H41A C41 H41B 108.3 . . ? N1 C42 C54 113.6(4) . . ? N1 C42 H42A 108.8 . . ? C54 C42 H42A 108.8 . . ? N1 C42 H42B 108.8 . . ? C54 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? N1 C43 C55 109.6(4) . . ? N1 C43 H43A 109.8 . . ? C55 C43 H43A 109.8 . . ? N1 C43 H43B 109.8 . . ? C55 C43 H43B 109.8 . . ? H43A C43 H43B 108.2 . . ? N5 C44 C56 108.5(4) . . ? N5 C44 H44A 110.0 . . ? C56 C44 H44A 110.0 . . ? N5 C44 H44B 110.0 . . ? C56 C44 H44B 110.0 . . ? H44A C44 H44B 108.4 . . ? N5 C45 C58 113.1(4) . . ? N5 C45 H45A 109.0 . . ? C58 C45 H45A 109.0 . . ? N5 C45 H45B 109.0 . . ? C58 C45 H45B 109.0 . . ? H45A C45 H45B 107.8 . . ? N5 C46 C57 109.5(4) . . ? N5 C46 H46A 109.8 . . ? C57 C46 H46A 109.8 . . ? N5 C46 H46B 109.8 . . ? C57 C46 H46B 109.8 . . ? H46A C46 H46B 108.2 . . ? N2 C53 C65 122.4(5) . . ? N2 C53 C41 114.3(4) . . ? C65 C53 C41 123.4(4) . . ? N3 C54 C69 122.6(5) . . ? N3 C54 C42 116.9(4) . . ? C69 C54 C42 120.4(5) . . ? N4 C55 C73 122.3(5) . . ? N4 C55 C43 115.5(4) . . ? C73 C55 C43 122.2(5) . . ? N6 C56 C80 122.9(5) . . ? N6 C56 C44 114.3(5) . . ? C80 C56 C44 122.8(5) . . ? N7 C57 C84 122.3(5) . . ? N7 C57 C46 115.5(4) . . ? C84 C57 C46 122.2(5) . . ? N8 C58 C85 122.3(5) . . ? N8 C58 C45 116.5(5) . . ? C85 C58 C45 121.1(5) . . ? C66 C65 C53 119.2(5) . . ? C66 C65 H65 120.4 . . ? C53 C65 H65 120.4 . . ? C65 C66 C67 118.6(5) . . ? C65 C66 H66 120.7 . . ? C67 C66 H66 120.7 . . ? C68 C67 C66 119.1(5) . . ? C68 C67 H67 120.4 . . ? C66 C67 H67 120.4 . . ? N2 C68 C67 122.9(5) . . ? N2 C68 H68 118.6 . . ? C67 C68 H68 118.6 . . ? C70 C69 C54 118.3(6) . . ? C70 C69 H69 120.8 . . ? C54 C69 H69 120.8 . . ? C69 C70 C71 119.7(6) . . ? C69 C70 H70 120.1 . . ? C71 C70 H70 120.1 . . ? C72 C71 C70 118.0(6) . . ? C72 C71 H71 121.0 . . ? C70 C71 H71 121.0 . . ? N3 C72 C71 123.5(5) . . ? N3 C72 H72 118.2 . . ? C71 C72 H72 118.2 . . ? C55 C73 C74 118.9(5) . . ? C55 C73 H73 120.5 . . ? C74 C73 H73 120.5 . . ? C75 C74 C73 119.5(5) . . ? C75 C74 H74 120.3 . . ? C73 C74 H74 120.3 . . ? C74 C75 C76 118.4(5) . . ? C74 C75 H75 120.8 . . ? C76 C75 H75 120.8 . . ? N4 C76 C75 122.2(5) . . ? N4 C76 H76 118.9 . . ? C75 C76 H76 118.9 . . ? N6 C77 C78 122.2(5) . . ? N6 C77 H77 118.9 . . ? C78 C77 H77 118.9 . . ? C79 C78 C77 119.3(5) . . ? C79 C78 H78 120.3 . . ? C77 C78 H78 120.3 . . ? C78 C79 C80 119.0(5) . . ? C78 C79 H79 120.5 . . ? C80 C79 H79 120.5 . . ? C56 C80 C79 118.3(5) . . ? C56 C80 H80 120.8 . . ? C79 C80 H80 120.8 . . ? N7 C81 C82 122.8(5) . . ? N7 C81 H81 118.6 . . ? C82 C81 H81 118.6 . . ? C83 C82 C81 119.3(5) . . ? C83 C82 H82 120.4 . . ? C81 C82 H82 120.4 . . ? C82 C83 C84 118.6(5) . . ? C82 C83 H83 120.7 . . ? C84 C83 H83 120.7 . . ? C57 C84 C83 119.3(5) . . ? C57 C84 H84 120.3 . . ? C83 C84 H84 120.3 . . ? C86 C85 C58 118.9(5) . . ? C86 C85 H85 120.5 . . ? C58 C85 H85 120.5 . . ? C85 C86 C87 119.2(5) . . ? C85 C86 H86 120.4 . . ? C87 C86 H86 120.4 . . ? C88 C87 C86 118.1(5) . . ? C88 C87 H87 120.9 . . ? C86 C87 H87 120.9 . . ? N8 C88 C87 123.3(5) . . ? N8 C88 H88 118.3 . . ? C87 C88 H88 118.3 . . ? O11 Mo3 O7 105.47(18) . . ? O11 Mo3 O8 105.8(2) . . ? O7 Mo3 O8 106.98(18) . . ? O11 Mo3 C11 93.5(2) . . ? O7 Mo3 C11 101.14(19) . . ? O8 Mo3 C11 139.72(19) . . ? O11 Mo3 C14 110.44(18) . . ? O7 Mo3 C14 138.02(17) . . ? O8 Mo3 C14 83.60(19) . . ? C11 Mo3 C14 56.4(2) . . ? O11 Mo3 C15 84.99(18) . . ? O7 Mo3 C15 135.3(2) . . ? O8 Mo3 C15 111.60(19) . . ? C11 Mo3 C15 34.2(2) . . ? C14 Mo3 C15 33.44(19) . . ? O11 Mo3 C13 141.30(18) . . ? O7 Mo3 C13 104.38(17) . . ? O8 Mo3 C13 88.21(19) . . ? C11 Mo3 C13 56.78(19) . . ? C14 Mo3 C13 34.13(16) . . ? C15 Mo3 C13 56.39(17) . . ? O11 Mo3 C12 127.1(2) . . ? O7 Mo3 C12 85.16(18) . . ? O8 Mo3 C12 120.47(18) . . ? C11 Mo3 C12 34.22(18) . . ? C14 Mo3 C12 55.95(18) . . ? C15 Mo3 C12 56.26(18) . . ? C13 Mo3 C12 33.66(19) . . ? O12 Mo4 O9 104.67(19) . . ? O12 Mo4 O10 105.57(18) . . ? O9 Mo4 O10 107.23(18) . . ? O12 Mo4 C16 91.84(19) . . ? O9 Mo4 C16 103.63(18) . . ? O10 Mo4 C16 138.94(18) . . ? O12 Mo4 C20 125.18(19) . . ? O9 Mo4 C20 86.41(17) . . ? O10 Mo4 C20 122.24(19) . . ? C16 Mo4 C20 34.28(19) . . ? O12 Mo4 C17 85.06(18) . . ? O9 Mo4 C17 137.86(18) . . ? O10 Mo4 C17 109.30(17) . . ? C16 Mo4 C17 34.35(18) . . ? C20 Mo4 C17 56.43(18) . . ? O12 Mo4 C19 140.95(17) . . ? O9 Mo4 C19 105.05(18) . . ? O10 Mo4 C19 89.10(18) . . ? C16 Mo4 C19 56.79(19) . . ? C20 Mo4 C19 34.15(19) . . ? C17 Mo4 C19 55.89(18) . . ? O12 Mo4 C18 111.03(18) . . ? O9 Mo4 C18 138.87(18) . . ? O10 Mo4 C18 82.48(17) . . ? C16 Mo4 C18 56.49(19) . . ? C20 Mo4 C18 56.53(18) . . ? C17 Mo4 C18 33.07(19) . . ? C19 Mo4 C18 34.04(18) . . ? O10 Fe3 O7 96.03(15) . . ? O10 Fe3 N10 112.30(16) . . ? O7 Fe3 N10 87.84(16) . . ? O10 Fe3 N11 95.48(16) . . ? O7 Fe3 N11 167.40(15) . . ? N10 Fe3 N11 92.53(16) . . ? O10 Fe3 N12 95.92(16) . . ? O7 Fe3 N12 94.16(15) . . ? N10 Fe3 N12 151.36(17) . . ? N11 Fe3 N12 79.55(16) . . ? O10 Fe3 N9 170.67(17) . . ? O7 Fe3 N9 89.90(15) . . ? N10 Fe3 N9 75.02(16) . . ? N11 Fe3 N9 78.05(16) . . ? N12 Fe3 N9 76.42(17) . . ? O8 Fe4 O9 94.05(16) . . ? O8 Fe4 N15 94.80(17) . . ? O9 Fe4 N15 169.70(18) . . ? O8 Fe4 N16 115.58(18) . . ? O9 Fe4 N16 88.30(15) . . ? N15 Fe4 N16 92.61(16) . . ? O8 Fe4 N13 168.22(16) . . ? O9 Fe4 N13 92.29(16) . . ? N15 Fe4 N13 78.10(17) . . ? N16 Fe4 N13 74.50(18) . . ? O8 Fe4 N14 93.53(19) . . ? O9 Fe4 N14 96.10(15) . . ? N15 Fe4 N14 78.12(16) . . ? N16 Fe4 N14 150.2(2) . . ? N13 Fe4 N14 75.91(19) . . ? C47 N9 C49 111.9(4) . . ? C47 N9 C48 111.0(4) . . ? C49 N9 C48 111.4(4) . . ? C47 N9 Fe3 106.9(3) . . ? C49 N9 Fe3 105.9(3) . . ? C48 N9 Fe3 109.5(3) . . ? C92 N10 C59 117.2(5) . . ? C92 N10 Fe3 127.3(4) . . ? C59 N10 Fe3 115.4(3) . . ? C60 N11 C96 118.3(5) . . ? C60 N11 Fe3 114.0(3) . . ? C96 N11 Fe3 124.3(4) . . ? C100 N12 C61 118.1(4) . . ? C100 N12 Fe3 124.8(3) . . ? C61 N12 Fe3 113.5(4) . . ? C50 N13 C52 113.0(4) . . ? C50 N13 C51 111.1(4) . . ? C52 N13 C51 109.7(5) . . ? C50 N13 Fe4 106.5(4) . . ? C52 N13 Fe4 106.6(4) . . ? C51 N13 Fe4 109.8(3) . . ? C62 N14 C104 119.0(5) . . ? C62 N14 Fe4 113.7(4) . . ? C104 N14 Fe4 123.1(4) . . ? C63 N15 C108 118.8(5) . . ? C63 N15 Fe4 114.4(3) . . ? C108 N15 Fe4 123.9(4) . . ? C112 N16 C64 117.9(5) . . ? C112 N16 Fe4 127.3(4) . . ? C64 N16 Fe4 114.9(4) . . ? Mo3 O7 Fe3 160.2(2) . . ? Mo3 O8 Fe4 157.2(2) . . ? Mo4 O9 Fe4 159.5(2) . . ? Mo4 O10 Fe3 153.1(2) . . ? C12 C11 C15 107.5(5) . . ? C12 C11 C31 126.9(5) . . ? C15 C11 C31 125.3(5) . . ? C12 C11 Mo3 74.4(3) . . ? C15 C11 Mo3 74.1(3) . . ? C31 C11 Mo3 121.5(4) . . ? C13 C12 C11 108.3(5) . . ? C13 C12 C32 125.7(5) . . ? C11 C12 C32 125.9(5) . . ? C13 C12 Mo3 72.9(3) . . ? C11 C12 Mo3 71.4(3) . . ? C32 C12 Mo3 119.0(4) . . ? C12 C13 C14 107.2(5) . . ? C12 C13 C33 127.6(5) . . ? C14 C13 C33 125.2(5) . . ? C12 C13 Mo3 73.5(3) . . ? C14 C13 Mo3 72.8(3) . . ? C33 C13 Mo3 119.2(4) . . ? C15 C14 C13 108.9(5) . . ? C15 C14 C34 126.8(5) . . ? C13 C14 C34 124.3(5) . . ? C15 C14 Mo3 73.4(3) . . ? C13 C14 Mo3 73.1(3) . . ? C34 C14 Mo3 119.3(4) . . ? C14 C15 C11 107.9(4) . . ? C14 C15 C35 128.1(6) . . ? C11 C15 C35 124.0(5) . . ? C14 C15 Mo3 73.1(3) . . ? C11 C15 Mo3 71.7(3) . . ? C35 C15 Mo3 119.3(4) . . ? C20 C16 C17 107.6(5) . . ? C20 C16 C36 126.9(5) . . ? C17 C16 C36 125.0(5) . . ? C20 C16 Mo4 73.7(3) . . ? C17 C16 Mo4 74.6(3) . . ? C36 C16 Mo4 123.3(4) . . ? C18 C17 C16 109.3(5) . . ? C18 C17 C37 127.4(5) . . ? C16 C17 C37 123.3(5) . . ? C18 C17 Mo4 75.0(3) . . ? C16 C17 Mo4 71.0(3) . . ? C37 C17 Mo4 120.3(3) . . ? C17 C18 C19 107.3(5) . . ? C17 C18 C38 128.1(5) . . ? C19 C18 C38 124.6(5) . . ? C17 C18 Mo4 71.9(3) . . ? C19 C18 Mo4 71.6(3) . . ? C38 C18 Mo4 121.6(4) . . ? C20 C19 C18 107.9(5) . . ? C20 C19 C39 127.2(5) . . ? C18 C19 C39 124.9(5) . . ? C20 C19 Mo4 71.9(3) . . ? C18 C19 Mo4 74.4(3) . . ? C39 C19 Mo4 120.1(3) . . ? C16 C20 C19 107.9(5) . . ? C16 C20 C40 127.9(5) . . ? C19 C20 C40 124.1(5) . . ? C16 C20 Mo4 72.0(3) . . ? C19 C20 Mo4 74.0(3) . . ? C40 C20 Mo4 120.9(3) . . ? C11 C31 H31A 109.5 . . ? C11 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C11 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C12 C32 H32A 109.5 . . ? C12 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C12 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C13 C33 H33A 109.5 . . ? C13 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C13 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C14 C34 H34A 109.5 . . ? C14 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C14 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C15 C35 H35A 109.5 . . ? C15 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C15 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C16 C36 H36A 109.5 . . ? C16 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C16 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C17 C37 H37A 109.5 . . ? C17 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C17 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C18 C38 H38A 109.5 . . ? C18 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C18 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C19 C39 H39A 109.5 . . ? C19 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C19 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C20 C40 H40A 109.5 . . ? C20 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C20 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N9 C47 C59 109.9(4) . . ? N9 C47 H47A 109.7 . . ? C59 C47 H47A 109.7 . . ? N9 C47 H47B 109.7 . . ? C59 C47 H47B 109.7 . . ? H47A C47 H47B 108.2 . . ? N9 C48 C60 113.6(4) . . ? N9 C48 H48A 108.8 . . ? C60 C48 H48A 108.8 . . ? N9 C48 H48B 108.8 . . ? C60 C48 H48B 108.8 . . ? H48A C48 H48B 107.7 . . ? N9 C49 C61 108.4(4) . . ? N9 C49 H49A 110.0 . . ? C61 C49 H49A 110.0 . . ? N9 C49 H49B 110.0 . . ? C61 C49 H49B 110.0 . . ? H49A C49 H49B 108.4 . . ? N13 C50 C62 109.6(5) . . ? N13 C50 H50A 109.8 . . ? C62 C50 H50A 109.8 . . ? N13 C50 H50B 109.8 . . ? C62 C50 H50B 109.8 . . ? H50A C50 H50B 108.2 . . ? N13 C51 C63 112.3(5) . . ? N13 C51 H51A 109.2 . . ? C63 C51 H51A 109.2 . . ? N13 C51 H51B 109.2 . . ? C63 C51 H51B 109.2 . . ? H51A C51 H51B 107.9 . . ? N13 C52 C64 109.7(5) . . ? N13 C52 H52A 109.7 . . ? C64 C52 H52A 109.7 . . ? N13 C52 H52B 109.7 . . ? C64 C52 H52B 109.7 . . ? H52A C52 H52B 108.2 . . ? N10 C59 C89 122.4(5) . . ? N10 C59 C47 115.6(5) . . ? C89 C59 C47 121.9(5) . . ? N11 C60 C93 122.0(5) . . ? N11 C60 C48 116.6(5) . . ? C93 C60 C48 121.4(5) . . ? N12 C61 C97 121.4(5) . . ? N12 C61 C49 114.9(4) . . ? C97 C61 C49 123.7(5) . . ? N14 C62 C101 122.6(6) . . ? N14 C62 C50 114.5(5) . . ? C101 C62 C50 122.9(6) . . ? N15 C63 C105 122.5(5) . . ? N15 C63 C51 117.0(5) . . ? C105 C63 C51 120.4(5) . . ? N16 C64 C109 122.0(6) . . ? N16 C64 C52 116.0(5) . . ? C109 C64 C52 122.0(6) . . ? C59 C89 C90 119.2(6) . . ? C59 C89 H89 120.4 . . ? C90 C89 H89 120.4 . . ? C91 C90 C89 118.6(6) . . ? C91 C90 H90 120.7 . . ? C89 C90 H90 120.7 . . ? C92 C91 C90 118.9(5) . . ? C92 C91 H91 120.6 . . ? C90 C91 H91 120.6 . . ? N10 C92 C91 123.6(5) . . ? N10 C92 H92 118.2 . . ? C91 C92 H92 118.2 . . ? C94 C93 C60 119.1(5) . . ? C94 C93 H93 120.4 . . ? C60 C93 H93 120.4 . . ? C93 C94 C95 119.2(6) . . ? C93 C94 H94 120.4 . . ? C95 C94 H94 120.4 . . ? C96 C95 C94 118.4(6) . . ? C96 C95 H95 120.8 . . ? C94 C95 H95 120.8 . . ? N11 C96 C95 123.0(5) . . ? N11 C96 H96 118.5 . . ? C95 C96 H96 118.5 . . ? C98 C97 C61 119.9(5) . . ? C98 C97 H97 120.1 . . ? C61 C97 H97 120.1 . . ? C97 C98 C99 118.9(5) . . ? C97 C98 H98 120.5 . . ? C99 C98 H98 120.5 . . ? C98 C99 C100 118.5(5) . . ? C98 C99 H99 120.8 . . ? C100 C99 H99 120.8 . . ? N12 C100 C99 123.3(5) . . ? N12 C100 H100 118.3 . . ? C99 C100 H100 118.4 . . ? C102 C101 C62 118.2(7) . . ? C102 C101 H101 120.9 . . ? C62 C101 H101 120.9 . . ? C103 C102 C101 119.2(6) . . ? C103 C102 H102 120.4 . . ? C101 C102 H102 120.4 . . ? C102 C103 C104 120.0(7) . . ? C102 C103 H103 120.0 . . ? C104 C103 H103 120.0 . . ? N14 C104 C103 121.1(7) . . ? N14 C104 H104 119.5 . . ? C103 C104 H104 119.5 . . ? C106 C105 C63 118.9(6) . . ? C106 C105 H105 120.5 . . ? C63 C105 H105 120.5 . . ? C105 C106 C107 118.9(5) . . ? C105 C106 H106 120.6 . . ? C107 C106 H106 120.6 . . ? C108 C107 C106 118.6(5) . . ? C108 C107 H107 120.7 . . ? C106 C107 H107 120.7 . . ? N15 C108 C107 122.2(6) . . ? N15 C108 H108 118.9 . . ? C107 C108 H108 118.9 . . ? C64 C109 C110 119.7(7) . . ? C64 C109 H109 120.1 . . ? C110 C109 H109 120.1 . . ? C111 C110 C109 118.3(6) . . ? C111 C110 H110 120.8 . . ? C109 C110 H110 120.8 . . ? C110 C111 C112 118.9(6) . . ? C110 C111 H111 120.5 . . ? C112 C111 H111 120.5 . . ? N16 C112 C111 123.0(6) . . ? N16 C112 H112 118.5 . . ? C111 C112 H112 118.5 . . ? O201 S200 O202 115.8(4) . . ? O201 S200 O203 115.1(3) . . ? O202 S200 O203 115.1(3) . . ? O201 S200 C200 102.7(4) . . ? O202 S200 C200 102.8(3) . . ? O203 S200 C200 102.6(3) . . ? F201 C200 F202 106.6(6) . . ? F201 C200 F203 106.8(6) . . ? F202 C200 F203 105.7(5) . . ? F201 C200 S200 112.7(5) . . ? F202 C200 S200 112.2(5) . . ? F203 C200 S200 112.4(5) . . ? O301 S300 O302 115.9(3) . . ? O301 S300 O303 114.7(2) . . ? O302 S300 O303 115.0(3) . . ? O301 S300 C300 103.0(3) . . ? O302 S300 C300 103.2(3) . . ? O303 S300 C300 102.4(3) . . ? F302 C300 F303 107.7(5) . . ? F302 C300 F301 106.7(5) . . ? F303 C300 F301 107.1(5) . . ? F302 C300 S300 111.6(4) . . ? F303 C300 S300 111.7(4) . . ? F301 C300 S300 111.7(4) . . ? N600 C601 C602 179.2(8) . . ? C601 C602 H60A 109.5 . . ? C601 C602 H60B 109.5 . . ? H60A C602 H60B 109.5 . . ? C601 C602 H60C 109.5 . . ? H60A C602 H60C 109.5 . . ? H60B C602 H60C 109.5 . . ? N700 C701 C702 178.9(7) . . ? C701 C702 H70A 109.5 . . ? C701 C702 H70B 109.5 . . ? H70A C702 H70B 109.5 . . ? C701 C702 H70C 109.5 . . ? H70A C702 H70C 109.5 . . ? H70B C702 H70C 109.5 . . ? N800 C801 C802 179.0(8) . . ? C801 C802 H80A 109.5 . . ? C801 C802 H80B 109.5 . . ? H80A C802 H80B 109.5 . . ? C801 C802 H80C 109.5 . . ? H80A C802 H80C 109.5 . . ? H80B C802 H80C 109.5 . . ? N900 C901 C902 172.7(16) . . ? C911 C912 H91A 109.5 . . ? C911 C912 H91B 109.5 . . ? H91A C912 H91B 109.5 . . ? C911 C912 H91C 109.5 . . ? H91A C912 H91C 109.5 . . ? H91B C912 H91C 109.5 . . ? O402 S400 O401 104.1(8) . . ? O402 S400 O403 140.1(8) . . ? O401 S400 O403 107.5(6) . . ? O402 S400 C400 98.7(7) . . ? O401 S400 C400 98.4(6) . . ? O403 S400 C400 100.1(5) . . ? F402 C400 F401 109.2(7) . . ? F402 C400 F403 96.9(8) . . ? F401 C400 F403 102.0(6) . . ? F402 C400 S400 119.4(7) . . ? F401 C400 S400 116.1(4) . . ? F403 C400 S400 110.1(6) . . ? S410 O412 C410 62.6(6) . . ? O413 S410 O411 122.0(14) . . ? O413 S410 O412 103.6(11) . . ? O411 S410 O412 127.5(15) . . ? O413 S410 C410 101.3(8) . . ? O411 S410 C410 117.1(13) . . ? O412 S410 C410 72.9(8) . . ? F412 C410 F411 105.8(11) . . ? F412 C410 F413 106.2(10) . . ? F411 C410 F413 104.6(10) . . ? F412 C410 S410 113.5(8) . . ? F411 C410 S410 113.5(8) . . ? F413 C410 S410 112.4(8) . . ? F412 C410 O412 97.6(10) . . ? F411 C410 O412 80.1(8) . . ? F413 C410 O412 153.1(9) . . ? O501 S500 O503 115.4(5) . . ? O501 S500 O502 111.7(7) . . ? O503 S500 O502 116.1(7) . . ? O501 S500 C500 101.7(5) . . ? O503 S500 C500 104.3(4) . . ? O502 S500 C500 105.5(6) . . ? F502 C500 F503 103.3(7) . . ? F502 C500 F501 108.8(8) . . ? F503 C500 F501 116.4(9) . . ? F502 C500 S500 112.9(5) . . ? F503 C500 S500 112.4(6) . . ? F501 C500 S500 103.3(7) . . ? O512 S510 O511 116.2(8) . . ? O512 S510 O513 113.2(3) . . ? O511 S510 O513 113.2(3) . . ? O512 S510 C510 105.1(6) . . ? O511 S510 C510 104.8(5) . . ? O513 S510 C510 102.6(7) . . ? F512 C510 F513 105.0(3) . . ? F512 C510 F511 114.1(9) . . ? F513 C510 F511 115.3(9) . . ? F512 C510 S510 110.1(9) . . ? F513 C510 S510 109.0(7) . . ? F511 C510 S510 103.4(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Mo1 O1 Fe1 -93.9(5) . . . . ? O2 Mo1 O1 Fe1 17.4(5) . . . . ? C1 Mo1 O1 Fe1 152.6(4) . . . . ? C5 Mo1 O1 Fe1 113.7(4) . . . . ? C2 Mo1 O1 Fe1 176.3(4) . . . . ? C4 Mo1 O1 Fe1 123.9(5) . . . . ? C3 Mo1 O1 Fe1 157.1(5) . . . . ? O4 Fe1 O1 Mo1 -45.1(5) . . . . ? N4 Fe1 O1 Mo1 -134.3(4) . . . . ? N3 Fe1 O1 Mo1 132.9(5) . . . . ? N2 Fe1 O1 Mo1 52.2(5) . . . . ? O5 Mo1 O2 Fe2 43.9(8) . . . . ? O1 Mo1 O2 Fe2 -68.4(8) . . . . ? C1 Mo1 O2 Fe2 140.0(8) . . . . ? C5 Mo1 O2 Fe2 170.8(8) . . . . ? C2 Mo1 O2 Fe2 141.3(7) . . . . ? C4 Mo1 O2 Fe2 -161.5(8) . . . . ? C3 Mo1 O2 Fe2 -167.5(7) . . . . ? O3 Fe2 O2 Mo1 101.5(8) . . . . ? N7 Fe2 O2 Mo1 -147.5(8) . . . . ? N5 Fe2 O2 Mo1 -73.2(8) . . . . ? N6 Fe2 O2 Mo1 2.3(8) . . . . ? O6 Mo2 O3 Fe2 -76.8(5) . . . . ? O4 Mo2 O3 Fe2 34.9(5) . . . . ? C8 Mo2 O3 Fe2 171.9(4) . . . . ? C9 Mo2 O3 Fe2 -166.9(4) . . . . ? C7 Mo2 O3 Fe2 131.1(4) . . . . ? C6 Mo2 O3 Fe2 139.6(5) . . . . ? C10 Mo2 O3 Fe2 172.6(5) . . . . ? O2 Fe2 O3 Mo2 -53.5(5) . . . . ? N8 Fe2 O3 Mo2 121.4(4) . . . . ? N7 Fe2 O3 Mo2 -143.9(4) . . . . ? N6 Fe2 O3 Mo2 42.7(5) . . . . ? O6 Mo2 O4 Fe1 37.0(5) . . . . ? O3 Mo2 O4 Fe1 -75.3(5) . . . . ? C8 Mo2 O4 Fe1 132.1(5) . . . . ? C9 Mo2 O4 Fe1 135.7(4) . . . . ? C7 Mo2 O4 Fe1 161.7(5) . . . . ? C6 Mo2 O4 Fe1 -169.7(5) . . . . ? C10 Mo2 O4 Fe1 -173.8(4) . . . . ? O1 Fe1 O4 Mo2 101.9(5) . . . . ? N4 Fe1 O4 Mo2 -146.2(5) . . . . ? N2 Fe1 O4 Mo2 4.6(5) . . . . ? N1 Fe1 O4 Mo2 -71.8(5) . . . . ? O4 Fe1 N1 C43 -51.5(3) . . . . ? N4 Fe1 N1 C43 35.3(3) . . . . ? N3 Fe1 N1 C43 129.5(3) . . . . ? N2 Fe1 N1 C43 -147.9(3) . . . . ? O4 Fe1 N1 C41 68.0(3) . . . . ? N4 Fe1 N1 C41 154.8(3) . . . . ? N3 Fe1 N1 C41 -111.0(3) . . . . ? N2 Fe1 N1 C41 -28.5(3) . . . . ? O4 Fe1 N1 C42 -171.3(3) . . . . ? N4 Fe1 N1 C42 -84.5(3) . . . . ? N3 Fe1 N1 C42 9.7(3) . . . . ? N2 Fe1 N1 C42 92.3(3) . . . . ? O1 Fe1 N2 C68 21.9(4) . . . . ? O4 Fe1 N2 C68 117.0(4) . . . . ? N4 Fe1 N2 C68 -145.7(4) . . . . ? N3 Fe1 N2 C68 -72.0(4) . . . . ? N1 Fe1 N2 C68 -152.2(4) . . . . ? O1 Fe1 N2 C53 179.0(4) . . . . ? O4 Fe1 N2 C53 -85.9(4) . . . . ? N4 Fe1 N2 C53 11.4(5) . . . . ? N3 Fe1 N2 C53 85.1(4) . . . . ? N1 Fe1 N2 C53 4.9(3) . . . . ? O1 Fe1 N3 C54 -167.5(4) . . . . ? N4 Fe1 N3 C54 80.4(4) . . . . ? N2 Fe1 N3 C54 -71.5(4) . . . . ? N1 Fe1 N3 C54 6.4(4) . . . . ? O1 Fe1 N3 C72 -5.1(5) . . . . ? N4 Fe1 N3 C72 -117.2(4) . . . . ? N2 Fe1 N3 C72 90.9(4) . . . . ? N1 Fe1 N3 C72 168.7(5) . . . . ? O1 Fe1 N4 C76 -13.4(5) . . . . ? O4 Fe1 N4 C76 -106.9(4) . . . . ? N3 Fe1 N4 C76 82.4(4) . . . . ? N2 Fe1 N4 C76 153.4(4) . . . . ? N1 Fe1 N4 C76 159.9(4) . . . . ? O1 Fe1 N4 C55 166.2(3) . . . . ? O4 Fe1 N4 C55 72.6(4) . . . . ? N3 Fe1 N4 C55 -98.1(4) . . . . ? N2 Fe1 N4 C55 -27.1(5) . . . . ? N1 Fe1 N4 C55 -20.5(3) . . . . ? O2 Fe2 N5 C46 -53.8(3) . . . . ? N8 Fe2 N5 C46 130.7(3) . . . . ? N7 Fe2 N5 C46 34.7(3) . . . . ? N6 Fe2 N5 C46 -148.8(3) . . . . ? O2 Fe2 N5 C44 65.9(3) . . . . ? N8 Fe2 N5 C44 -109.6(3) . . . . ? N7 Fe2 N5 C44 154.4(3) . . . . ? N6 Fe2 N5 C44 -29.1(3) . . . . ? O2 Fe2 N5 C45 -172.8(3) . . . . ? N8 Fe2 N5 C45 11.7(3) . . . . ? N7 Fe2 N5 C45 -84.3(3) . . . . ? N6 Fe2 N5 C45 92.2(3) . . . . ? O3 Fe2 N6 C77 23.2(4) . . . . ? O2 Fe2 N6 C77 117.3(4) . . . . ? N8 Fe2 N6 C77 -70.0(4) . . . . ? N7 Fe2 N6 C77 -144.5(4) . . . . ? N5 Fe2 N6 C77 -151.2(4) . . . . ? O3 Fe2 N6 C56 179.5(3) . . . . ? O2 Fe2 N6 C56 -86.4(4) . . . . ? N8 Fe2 N6 C56 86.2(4) . . . . ? N7 Fe2 N6 C56 11.7(5) . . . . ? N5 Fe2 N6 C56 5.1(3) . . . . ? O3 Fe2 N7 C81 -14.4(5) . . . . ? O2 Fe2 N7 C81 -107.6(5) . . . . ? N8 Fe2 N7 C81 81.9(5) . . . . ? N5 Fe2 N7 C81 159.3(5) . . . . ? N6 Fe2 N7 C81 152.6(4) . . . . ? O3 Fe2 N7 C57 167.9(4) . . . . ? O2 Fe2 N7 C57 74.7(4) . . . . ? N8 Fe2 N7 C57 -95.8(4) . . . . ? N5 Fe2 N7 C57 -18.4(4) . . . . ? N6 Fe2 N7 C57 -25.1(6) . . . . ? O3 Fe2 N8 C58 -169.2(4) . . . . ? N7 Fe2 N8 C58 79.5(4) . . . . ? N5 Fe2 N8 C58 6.0(4) . . . . ? N6 Fe2 N8 C58 -71.2(4) . . . . ? O3 Fe2 N8 C88 -7.8(4) . . . . ? N7 Fe2 N8 C88 -119.2(4) . . . . ? N5 Fe2 N8 C88 167.4(4) . . . . ? N6 Fe2 N8 C88 90.2(4) . . . . ? O5 Mo1 C1 C2 -76.0(3) . . . . ? O2 Mo1 C1 C2 178.5(3) . . . . ? O1 Mo1 C1 C2 42.0(4) . . . . ? C5 Mo1 C1 C2 114.6(5) . . . . ? C4 Mo1 C1 C2 77.2(3) . . . . ? C3 Mo1 C1 C2 36.7(3) . . . . ? O5 Mo1 C1 C5 169.4(3) . . . . ? O2 Mo1 C1 C5 63.9(3) . . . . ? O1 Mo1 C1 C5 -72.5(4) . . . . ? C2 Mo1 C1 C5 -114.6(5) . . . . ? C4 Mo1 C1 C5 -37.3(3) . . . . ? C3 Mo1 C1 C5 -77.8(3) . . . . ? O5 Mo1 C1 C21 45.0(5) . . . . ? O2 Mo1 C1 C21 -60.5(5) . . . . ? O1 Mo1 C1 C21 163.0(4) . . . . ? C5 Mo1 C1 C21 -124.4(6) . . . . ? C2 Mo1 C1 C21 121.0(6) . . . . ? C4 Mo1 C1 C21 -161.8(5) . . . . ? C3 Mo1 C1 C21 157.8(5) . . . . ? C5 C1 C2 C3 0.0(6) . . . . ? C21 C1 C2 C3 174.3(5) . . . . ? Mo1 C1 C2 C3 -66.2(4) . . . . ? C5 C1 C2 C22 -179.5(5) . . . . ? C21 C1 C2 C22 -5.2(8) . . . . ? Mo1 C1 C2 C22 114.3(5) . . . . ? C5 C1 C2 Mo1 66.2(3) . . . . ? C21 C1 C2 Mo1 -119.5(5) . . . . ? O5 Mo1 C2 C3 -141.4(3) . . . . ? O2 Mo1 C2 C3 113.4(4) . . . . ? O1 Mo1 C2 C3 -36.4(4) . . . . ? C1 Mo1 C2 C3 115.6(5) . . . . ? C5 Mo1 C2 C3 77.5(3) . . . . ? C4 Mo1 C2 C3 36.5(3) . . . . ? O5 Mo1 C2 C1 103.0(3) . . . . ? O2 Mo1 C2 C1 -2.2(5) . . . . ? O1 Mo1 C2 C1 -152.0(3) . . . . ? C5 Mo1 C2 C1 -38.1(3) . . . . ? C4 Mo1 C2 C1 -79.0(3) . . . . ? C3 Mo1 C2 C1 -115.6(5) . . . . ? O5 Mo1 C2 C22 -16.6(4) . . . . ? O2 Mo1 C2 C22 -121.8(4) . . . . ? O1 Mo1 C2 C22 88.4(5) . . . . ? C1 Mo1 C2 C22 -119.6(6) . . . . ? C5 Mo1 C2 C22 -157.7(5) . . . . ? C4 Mo1 C2 C22 161.3(5) . . . . ? C3 Mo1 C2 C22 124.8(6) . . . . ? C1 C2 C3 C4 0.6(6) . . . . ? C22 C2 C3 C4 -179.9(5) . . . . ? Mo1 C2 C3 C4 -63.3(4) . . . . ? C1 C2 C3 C23 179.7(5) . . . . ? C22 C2 C3 C23 -0.8(9) . . . . ? Mo1 C2 C3 C23 115.8(6) . . . . ? C1 C2 C3 Mo1 63.9(3) . . . . ? C22 C2 C3 Mo1 -116.6(5) . . . . ? O5 Mo1 C3 C2 41.4(4) . . . . ? O2 Mo1 C3 C2 -106.0(4) . . . . ? O1 Mo1 C3 C2 145.9(3) . . . . ? C1 Mo1 C3 C2 -37.7(3) . . . . ? C5 Mo1 C3 C2 -79.6(3) . . . . ? C4 Mo1 C3 C2 -116.6(5) . . . . ? O5 Mo1 C3 C4 158.0(3) . . . . ? O2 Mo1 C3 C4 10.6(4) . . . . ? O1 Mo1 C3 C4 -97.5(3) . . . . ? C1 Mo1 C3 C4 78.9(3) . . . . ? C5 Mo1 C3 C4 37.0(3) . . . . ? C2 Mo1 C3 C4 116.6(5) . . . . ? O5 Mo1 C3 C23 -81.5(5) . . . . ? O2 Mo1 C3 C23 131.1(4) . . . . ? O1 Mo1 C3 C23 22.9(5) . . . . ? C1 Mo1 C3 C23 -160.6(5) . . . . ? C5 Mo1 C3 C23 157.5(5) . . . . ? C2 Mo1 C3 C23 -122.9(6) . . . . ? C4 Mo1 C3 C23 120.5(6) . . . . ? C2 C3 C4 C5 -1.0(6) . . . . ? C23 C3 C4 C5 179.9(5) . . . . ? Mo1 C3 C4 C5 -64.1(4) . . . . ? C2 C3 C4 C24 -179.0(5) . . . . ? C23 C3 C4 C24 1.9(9) . . . . ? Mo1 C3 C4 C24 117.8(5) . . . . ? C2 C3 C4 Mo1 63.2(4) . . . . ? C23 C3 C4 Mo1 -115.9(5) . . . . ? O5 Mo1 C4 C5 82.9(4) . . . . ? O2 Mo1 C4 C5 -56.6(3) . . . . ? O1 Mo1 C4 C5 -164.1(3) . . . . ? C1 Mo1 C4 C5 38.2(3) . . . . ? C2 Mo1 C4 C5 79.7(3) . . . . ? C3 Mo1 C4 C5 116.2(4) . . . . ? O5 Mo1 C4 C3 -33.3(4) . . . . ? O2 Mo1 C4 C3 -172.8(3) . . . . ? O1 Mo1 C4 C3 79.7(3) . . . . ? C1 Mo1 C4 C3 -78.0(3) . . . . ? C5 Mo1 C4 C3 -116.2(4) . . . . ? C2 Mo1 C4 C3 -36.5(3) . . . . ? O5 Mo1 C4 C24 -155.9(4) . . . . ? O2 Mo1 C4 C24 64.5(5) . . . . ? O1 Mo1 C4 C24 -43.0(5) . . . . ? C1 Mo1 C4 C24 159.3(5) . . . . ? C5 Mo1 C4 C24 121.1(6) . . . . ? C2 Mo1 C4 C24 -159.2(6) . . . . ? C3 Mo1 C4 C24 -122.7(6) . . . . ? C3 C4 C5 C1 0.9(6) . . . . ? C24 C4 C5 C1 179.0(5) . . . . ? Mo1 C4 C5 C1 -65.0(3) . . . . ? C3 C4 C5 C25 -176.1(5) . . . . ? C24 C4 C5 C25 1.9(8) . . . . ? Mo1 C4 C5 C25 117.9(5) . . . . ? C3 C4 C5 Mo1 66.0(4) . . . . ? C24 C4 C5 Mo1 -116.0(5) . . . . ? C2 C1 C5 C4 -0.6(6) . . . . ? C21 C1 C5 C4 -174.6(5) . . . . ? Mo1 C1 C5 C4 66.5(3) . . . . ? C2 C1 C5 C25 176.4(5) . . . . ? C21 C1 C5 C25 2.4(9) . . . . ? Mo1 C1 C5 C25 -116.5(5) . . . . ? C2 C1 C5 Mo1 -67.1(3) . . . . ? C21 C1 C5 Mo1 118.9(5) . . . . ? O5 Mo1 C5 C4 -127.9(3) . . . . ? O2 Mo1 C5 C4 126.6(3) . . . . ? O1 Mo1 C5 C4 18.5(3) . . . . ? C1 Mo1 C5 C4 -114.7(4) . . . . ? C2 Mo1 C5 C4 -77.0(3) . . . . ? C3 Mo1 C5 C4 -36.6(3) . . . . ? O5 Mo1 C5 C1 -13.2(4) . . . . ? O2 Mo1 C5 C1 -118.7(3) . . . . ? O1 Mo1 C5 C1 133.2(3) . . . . ? C2 Mo1 C5 C1 37.7(3) . . . . ? C4 Mo1 C5 C1 114.7(4) . . . . ? C3 Mo1 C5 C1 78.1(3) . . . . ? O5 Mo1 C5 C25 109.7(4) . . . . ? O2 Mo1 C5 C25 4.1(4) . . . . ? O1 Mo1 C5 C25 -104.0(4) . . . . ? C1 Mo1 C5 C25 122.8(6) . . . . ? C2 Mo1 C5 C25 160.6(5) . . . . ? C4 Mo1 C5 C25 -122.5(6) . . . . ? C3 Mo1 C5 C25 -159.1(5) . . . . ? O6 Mo2 C6 C10 -38.4(4) . . . . ? O4 Mo2 C6 C10 -175.0(3) . . . . ? O3 Mo2 C6 C10 76.9(3) . . . . ? C8 Mo2 C6 C10 -78.1(3) . . . . ? C9 Mo2 C6 C10 -36.8(3) . . . . ? C7 Mo2 C6 C10 -116.0(4) . . . . ? O6 Mo2 C6 C7 77.5(4) . . . . ? O4 Mo2 C6 C7 -59.0(3) . . . . ? O3 Mo2 C6 C7 -167.2(3) . . . . ? C8 Mo2 C6 C7 37.8(3) . . . . ? C9 Mo2 C6 C7 79.1(3) . . . . ? C10 Mo2 C6 C7 116.0(4) . . . . ? O6 Mo2 C6 C26 -159.6(4) . . . . ? O4 Mo2 C6 C26 63.8(5) . . . . ? O3 Mo2 C6 C26 -44.3(5) . . . . ? C8 Mo2 C6 C26 160.7(5) . . . . ? C9 Mo2 C6 C26 -158.0(5) . . . . ? C7 Mo2 C6 C26 122.9(6) . . . . ? C10 Mo2 C6 C26 -121.2(6) . . . . ? C10 C6 C7 C8 1.5(6) . . . . ? C26 C6 C7 C8 -179.4(5) . . . . ? Mo2 C6 C7 C8 -63.6(3) . . . . ? C10 C6 C7 C27 -177.4(5) . . . . ? C26 C6 C7 C27 1.6(8) . . . . ? Mo2 C6 C7 C27 117.4(5) . . . . ? C10 C6 C7 Mo2 65.1(3) . . . . ? C26 C6 C7 Mo2 -115.8(5) . . . . ? O6 Mo2 C7 C6 -131.5(3) . . . . ? O4 Mo2 C7 C6 123.4(3) . . . . ? O3 Mo2 C7 C6 15.3(3) . . . . ? C8 Mo2 C7 C6 -115.1(4) . . . . ? C9 Mo2 C7 C6 -77.4(3) . . . . ? C10 Mo2 C7 C6 -36.9(3) . . . . ? O6 Mo2 C7 C8 -16.4(4) . . . . ? O4 Mo2 C7 C8 -121.5(3) . . . . ? O3 Mo2 C7 C8 130.4(3) . . . . ? C9 Mo2 C7 C8 37.6(3) . . . . ? C6 Mo2 C7 C8 115.1(4) . . . . ? C10 Mo2 C7 C8 78.2(3) . . . . ? O6 Mo2 C7 C27 106.3(4) . . . . ? O4 Mo2 C7 C27 1.3(4) . . . . ? O3 Mo2 C7 C27 -106.9(4) . . . . ? C8 Mo2 C7 C27 122.7(6) . . . . ? C9 Mo2 C7 C27 160.4(5) . . . . ? C6 Mo2 C7 C27 -122.2(5) . . . . ? C10 Mo2 C7 C27 -159.1(5) . . . . ? C6 C7 C8 C9 -1.9(6) . . . . ? C27 C7 C8 C9 177.1(5) . . . . ? Mo2 C7 C8 C9 -67.2(4) . . . . ? C6 C7 C8 C28 -177.1(5) . . . . ? C27 C7 C8 C28 1.8(9) . . . . ? Mo2 C7 C8 C28 117.6(5) . . . . ? C6 C7 C8 Mo2 65.3(3) . . . . ? C27 C7 C8 Mo2 -115.7(5) . . . . ? O6 Mo2 C8 C9 -78.7(3) . . . . ? O4 Mo2 C8 C9 175.6(3) . . . . ? O3 Mo2 C8 C9 37.5(4) . . . . ? C7 Mo2 C8 C9 114.7(4) . . . . ? C6 Mo2 C8 C9 77.5(3) . . . . ? C10 Mo2 C8 C9 36.7(3) . . . . ? O6 Mo2 C8 C7 166.6(3) . . . . ? O4 Mo2 C8 C7 60.9(3) . . . . ? O3 Mo2 C8 C7 -77.2(4) . . . . ? C9 Mo2 C8 C7 -114.7(4) . . . . ? C6 Mo2 C8 C7 -37.2(3) . . . . ? C10 Mo2 C8 C7 -78.0(3) . . . . ? O6 Mo2 C8 C28 41.9(5) . . . . ? O4 Mo2 C8 C28 -63.8(5) . . . . ? O3 Mo2 C8 C28 158.1(4) . . . . ? C9 Mo2 C8 C28 120.6(6) . . . . ? C7 Mo2 C8 C28 -124.7(6) . . . . ? C6 Mo2 C8 C28 -161.9(5) . . . . ? C10 Mo2 C8 C28 157.4(5) . . . . ? C7 C8 C9 C10 1.5(6) . . . . ? C28 C8 C9 C10 177.0(5) . . . . ? Mo2 C8 C9 C10 -65.9(3) . . . . ? C7 C8 C9 C29 -179.2(5) . . . . ? C28 C8 C9 C29 -3.8(8) . . . . ? Mo2 C8 C9 C29 113.3(5) . . . . ? C7 C8 C9 Mo2 67.4(3) . . . . ? C28 C8 C9 Mo2 -117.1(5) . . . . ? O6 Mo2 C9 C10 -144.0(3) . . . . ? O4 Mo2 C9 C10 109.5(3) . . . . ? O3 Mo2 C9 C10 -39.1(3) . . . . ? C8 Mo2 C9 C10 115.8(4) . . . . ? C7 Mo2 C9 C10 77.9(3) . . . . ? C6 Mo2 C9 C10 37.0(3) . . . . ? O6 Mo2 C9 C8 100.2(3) . . . . ? O4 Mo2 C9 C8 -6.3(4) . . . . ? O3 Mo2 C9 C8 -154.9(3) . . . . ? C7 Mo2 C9 C8 -37.9(3) . . . . ? C6 Mo2 C9 C8 -78.8(3) . . . . ? C10 Mo2 C9 C8 -115.8(4) . . . . ? O6 Mo2 C9 C29 -19.4(4) . . . . ? O4 Mo2 C9 C29 -125.9(4) . . . . ? O3 Mo2 C9 C29 85.5(4) . . . . ? C8 Mo2 C9 C29 -119.5(5) . . . . ? C7 Mo2 C9 C29 -157.4(5) . . . . ? C6 Mo2 C9 C29 161.6(5) . . . . ? C10 Mo2 C9 C29 124.7(6) . . . . ? C8 C9 C10 C6 -0.6(6) . . . . ? C29 C9 C10 C6 -179.8(5) . . . . ? Mo2 C9 C10 C6 -64.7(3) . . . . ? C8 C9 C10 C30 -179.3(5) . . . . ? C29 C9 C10 C30 1.5(9) . . . . ? Mo2 C9 C10 C30 116.6(5) . . . . ? C8 C9 C10 Mo2 64.1(3) . . . . ? C29 C9 C10 Mo2 -115.1(5) . . . . ? C7 C6 C10 C9 -0.6(6) . . . . ? C26 C6 C10 C9 -179.7(5) . . . . ? Mo2 C6 C10 C9 64.1(3) . . . . ? C7 C6 C10 C30 178.2(5) . . . . ? C26 C6 C10 C30 -0.9(8) . . . . ? Mo2 C6 C10 C30 -117.1(5) . . . . ? C7 C6 C10 Mo2 -64.7(3) . . . . ? C26 C6 C10 Mo2 116.2(5) . . . . ? O6 Mo2 C10 C9 39.0(4) . . . . ? O4 Mo2 C10 C9 -108.8(3) . . . . ? O3 Mo2 C10 C9 143.1(3) . . . . ? C8 Mo2 C10 C9 -37.4(3) . . . . ? C7 Mo2 C10 C9 -79.0(3) . . . . ? C6 Mo2 C10 C9 -116.0(4) . . . . ? O6 Mo2 C10 C6 155.0(3) . . . . ? O4 Mo2 C10 C6 7.2(4) . . . . ? O3 Mo2 C10 C6 -100.9(3) . . . . ? C8 Mo2 C10 C6 78.6(3) . . . . ? C9 Mo2 C10 C6 116.0(4) . . . . ? C7 Mo2 C10 C6 37.0(3) . . . . ? O6 Mo2 C10 C30 -84.5(4) . . . . ? O4 Mo2 C10 C30 127.7(4) . . . . ? O3 Mo2 C10 C30 19.6(4) . . . . ? C8 Mo2 C10 C30 -160.9(5) . . . . ? C9 Mo2 C10 C30 -123.5(5) . . . . ? C7 Mo2 C10 C30 157.6(5) . . . . ? C6 Mo2 C10 C30 120.5(5) . . . . ? C43 N1 C41 C53 162.5(4) . . . . ? C42 N1 C41 C53 -72.1(5) . . . . ? Fe1 N1 C41 C53 47.3(4) . . . . ? C43 N1 C42 C54 -140.1(4) . . . . ? C41 N1 C42 C54 93.7(5) . . . . ? Fe1 N1 C42 C54 -23.3(5) . . . . ? C41 N1 C43 C55 -160.8(4) . . . . ? C42 N1 C43 C55 73.3(5) . . . . ? Fe1 N1 C43 C55 -45.7(4) . . . . ? C46 N5 C44 C56 164.7(4) . . . . ? C45 N5 C44 C56 -71.2(5) . . . . ? Fe2 N5 C44 C56 48.3(5) . . . . ? C46 N5 C45 C58 -143.2(4) . . . . ? C44 N5 C45 C58 92.0(5) . . . . ? Fe2 N5 C45 C58 -26.5(5) . . . . ? C44 N5 C46 C57 -163.6(4) . . . . ? C45 N5 C46 C57 71.4(5) . . . . ? Fe2 N5 C46 C57 -46.8(5) . . . . ? C68 N2 C53 C65 0.1(8) . . . . ? Fe1 N2 C53 C65 -158.5(4) . . . . ? C68 N2 C53 C41 179.2(4) . . . . ? Fe1 N2 C53 C41 20.5(5) . . . . ? N1 C41 C53 N2 -46.9(6) . . . . ? N1 C41 C53 C65 132.1(5) . . . . ? C72 N3 C54 C69 -3.0(8) . . . . ? Fe1 N3 C54 C69 160.8(5) . . . . ? C72 N3 C54 C42 174.3(5) . . . . ? Fe1 N3 C54 C42 -21.9(6) . . . . ? N1 C42 C54 N3 31.0(7) . . . . ? N1 C42 C54 C69 -151.6(5) . . . . ? C76 N4 C55 C73 1.6(8) . . . . ? Fe1 N4 C55 C73 -178.0(4) . . . . ? C76 N4 C55 C43 -179.5(5) . . . . ? Fe1 N4 C55 C43 0.9(6) . . . . ? N1 C43 C55 N4 31.3(6) . . . . ? N1 C43 C55 C73 -149.7(5) . . . . ? C77 N6 C56 C80 -1.1(8) . . . . ? Fe2 N6 C56 C80 -158.8(4) . . . . ? C77 N6 C56 C44 178.1(5) . . . . ? Fe2 N6 C56 C44 20.4(5) . . . . ? N5 C44 C56 N6 -46.9(6) . . . . ? N5 C44 C56 C80 132.3(5) . . . . ? C81 N7 C57 C84 0.0(8) . . . . ? Fe2 N7 C57 C84 178.0(4) . . . . ? C81 N7 C57 C46 179.8(5) . . . . ? Fe2 N7 C57 C46 -2.2(6) . . . . ? N5 C46 C57 N7 33.7(7) . . . . ? N5 C46 C57 C84 -146.5(5) . . . . ? C88 N8 C58 C85 -3.1(8) . . . . ? Fe2 N8 C58 C85 159.6(4) . . . . ? C88 N8 C58 C45 174.0(4) . . . . ? Fe2 N8 C58 C45 -23.2(6) . . . . ? N5 C45 C58 N8 34.3(6) . . . . ? N5 C45 C58 C85 -148.5(5) . . . . ? N2 C53 C65 C66 0.1(9) . . . . ? C41 C53 C65 C66 -178.9(5) . . . . ? C53 C65 C66 C67 -0.4(9) . . . . ? C65 C66 C67 C68 0.6(9) . . . . ? C53 N2 C68 C67 0.0(8) . . . . ? Fe1 N2 C68 C67 156.4(4) . . . . ? C66 C67 C68 N2 -0.4(9) . . . . ? N3 C54 C69 C70 3.0(9) . . . . ? C42 C54 C69 C70 -174.2(6) . . . . ? C54 C69 C70 C71 0.0(10) . . . . ? C69 C70 C71 C72 -2.7(10) . . . . ? C54 N3 C72 C71 0.1(8) . . . . ? Fe1 N3 C72 C71 -161.8(5) . . . . ? C70 C71 C72 N3 2.8(10) . . . . ? N4 C55 C73 C74 -0.8(8) . . . . ? C43 C55 C73 C74 -179.7(5) . . . . ? C55 C73 C74 C75 -0.7(9) . . . . ? C73 C74 C75 C76 1.4(9) . . . . ? C55 N4 C76 C75 -0.8(8) . . . . ? Fe1 N4 C76 C75 178.7(4) . . . . ? C74 C75 C76 N4 -0.6(9) . . . . ? C56 N6 C77 C78 1.3(8) . . . . ? Fe2 N6 C77 C78 156.5(4) . . . . ? N6 C77 C78 C79 -0.7(9) . . . . ? C77 C78 C79 C80 -0.1(9) . . . . ? N6 C56 C80 C79 0.3(8) . . . . ? C44 C56 C80 C79 -178.8(5) . . . . ? C78 C79 C80 C56 0.3(9) . . . . ? C57 N7 C81 C82 -1.2(8) . . . . ? Fe2 N7 C81 C82 -178.9(4) . . . . ? N7 C81 C82 C83 1.7(9) . . . . ? C81 C82 C83 C84 -0.8(9) . . . . ? N7 C57 C84 C83 0.7(9) . . . . ? C46 C57 C84 C83 -179.1(6) . . . . ? C82 C83 C84 C57 -0.3(9) . . . . ? N8 C58 C85 C86 4.5(8) . . . . ? C45 C58 C85 C86 -172.5(5) . . . . ? C58 C85 C86 C87 -1.9(9) . . . . ? C85 C86 C87 C88 -1.8(8) . . . . ? C58 N8 C88 C87 -0.8(8) . . . . ? Fe2 N8 C88 C87 -161.5(4) . . . . ? C86 C87 C88 N8 3.2(8) . . . . ? O7 Fe3 N9 C47 54.5(3) . . . . ? N10 Fe3 N9 C47 -33.3(3) . . . . ? N11 Fe3 N9 C47 -129.2(3) . . . . ? N12 Fe3 N9 C47 148.8(3) . . . . ? O7 Fe3 N9 C49 -65.0(3) . . . . ? N10 Fe3 N9 C49 -152.7(3) . . . . ? N11 Fe3 N9 C49 111.3(3) . . . . ? N12 Fe3 N9 C49 29.4(3) . . . . ? O7 Fe3 N9 C48 174.8(3) . . . . ? N10 Fe3 N9 C48 87.0(3) . . . . ? N11 Fe3 N9 C48 -8.9(3) . . . . ? N12 Fe3 N9 C48 -90.9(3) . . . . ? O10 Fe3 N10 C92 11.0(5) . . . . ? O7 Fe3 N10 C92 106.6(4) . . . . ? N11 Fe3 N10 C92 -86.0(4) . . . . ? N12 Fe3 N10 C92 -158.6(4) . . . . ? N9 Fe3 N10 C92 -162.9(5) . . . . ? O10 Fe3 N10 C59 -168.4(3) . . . . ? O7 Fe3 N10 C59 -72.8(4) . . . . ? N11 Fe3 N10 C59 94.6(4) . . . . ? N12 Fe3 N10 C59 22.0(6) . . . . ? N9 Fe3 N10 C59 17.7(4) . . . . ? O10 Fe3 N11 C60 164.5(4) . . . . ? O7 Fe3 N11 C60 8.6(10) . . . . ? N10 Fe3 N11 C60 -82.8(4) . . . . ? N12 Fe3 N11 C60 69.5(4) . . . . ? N9 Fe3 N11 C60 -8.7(4) . . . . ? O10 Fe3 N11 C96 5.6(4) . . . . ? O7 Fe3 N11 C96 -150.3(7) . . . . ? N10 Fe3 N11 C96 118.3(4) . . . . ? N12 Fe3 N11 C96 -89.4(4) . . . . ? N9 Fe3 N11 C96 -167.6(4) . . . . ? O10 Fe3 N12 C100 -22.7(4) . . . . ? O7 Fe3 N12 C100 -119.2(4) . . . . ? N10 Fe3 N12 C100 147.7(4) . . . . ? N11 Fe3 N12 C100 71.8(4) . . . . ? N9 Fe3 N12 C100 151.9(4) . . . . ? O10 Fe3 N12 C61 179.4(3) . . . . ? O7 Fe3 N12 C61 82.8(4) . . . . ? N10 Fe3 N12 C61 -10.3(5) . . . . ? N11 Fe3 N12 C61 -86.1(4) . . . . ? N9 Fe3 N12 C61 -6.0(3) . . . . ? O8 Fe4 N13 C50 54.6(9) . . . . ? O9 Fe4 N13 C50 -68.0(3) . . . . ? N15 Fe4 N13 C50 108.3(3) . . . . ? N16 Fe4 N13 C50 -155.6(3) . . . . ? N14 Fe4 N13 C50 27.7(3) . . . . ? O8 Fe4 N13 C52 175.5(7) . . . . ? O9 Fe4 N13 C52 53.0(3) . . . . ? N15 Fe4 N13 C52 -130.8(4) . . . . ? N16 Fe4 N13 C52 -34.6(3) . . . . ? N14 Fe4 N13 C52 148.7(4) . . . . ? O8 Fe4 N13 C51 -65.7(9) . . . . ? O9 Fe4 N13 C51 171.7(3) . . . . ? N15 Fe4 N13 C51 -12.0(3) . . . . ? N16 Fe4 N13 C51 84.1(3) . . . . ? N14 Fe4 N13 C51 -92.6(3) . . . . ? O8 Fe4 N14 C62 -179.5(4) . . . . ? O9 Fe4 N14 C62 86.0(4) . . . . ? N15 Fe4 N14 C62 -85.3(4) . . . . ? N16 Fe4 N14 C62 -11.2(6) . . . . ? N13 Fe4 N14 C62 -4.8(4) . . . . ? O8 Fe4 N14 C104 -22.9(5) . . . . ? O9 Fe4 N14 C104 -117.3(4) . . . . ? N15 Fe4 N14 C104 71.3(4) . . . . ? N16 Fe4 N14 C104 145.4(4) . . . . ? N13 Fe4 N14 C104 151.8(5) . . . . ? O8 Fe4 N15 C63 164.8(4) . . . . ? O9 Fe4 N15 C63 15.6(11) . . . . ? N16 Fe4 N15 C63 -79.2(4) . . . . ? N13 Fe4 N15 C63 -5.7(4) . . . . ? N14 Fe4 N15 C63 72.2(4) . . . . ? O8 Fe4 N15 C108 4.6(4) . . . . ? O9 Fe4 N15 C108 -144.6(8) . . . . ? N16 Fe4 N15 C108 120.6(4) . . . . ? N13 Fe4 N15 C108 -165.9(4) . . . . ? N14 Fe4 N15 C108 -88.0(4) . . . . ? O8 Fe4 N16 C112 12.6(5) . . . . ? O9 Fe4 N16 C112 106.3(5) . . . . ? N15 Fe4 N16 C112 -84.0(5) . . . . ? N13 Fe4 N16 C112 -160.9(5) . . . . ? N14 Fe4 N16 C112 -154.4(4) . . . . ? O8 Fe4 N16 C64 -166.9(4) . . . . ? O9 Fe4 N16 C64 -73.2(4) . . . . ? N15 Fe4 N16 C64 96.5(4) . . . . ? N13 Fe4 N16 C64 19.6(4) . . . . ? N14 Fe4 N16 C64 26.1(6) . . . . ? O11 Mo3 O7 Fe3 -53.8(7) . . . . ? O8 Mo3 O7 Fe3 58.5(7) . . . . ? C11 Mo3 O7 Fe3 -150.7(6) . . . . ? C14 Mo3 O7 Fe3 158.0(6) . . . . ? C15 Mo3 O7 Fe3 -152.5(6) . . . . ? C13 Mo3 O7 Fe3 151.1(6) . . . . ? C12 Mo3 O7 Fe3 178.9(7) . . . . ? O10 Fe3 O7 Mo3 -89.8(7) . . . . ? N10 Fe3 O7 Mo3 158.0(7) . . . . ? N11 Fe3 O7 Mo3 66.1(11) . . . . ? N12 Fe3 O7 Mo3 6.6(7) . . . . ? N9 Fe3 O7 Mo3 83.0(7) . . . . ? O11 Mo3 O8 Fe4 102.5(6) . . . . ? O7 Mo3 O8 Fe4 -9.6(6) . . . . ? C11 Mo3 O8 Fe4 -141.8(5) . . . . ? C14 Mo3 O8 Fe4 -148.0(6) . . . . ? C15 Mo3 O8 Fe4 -166.6(5) . . . . ? C13 Mo3 O8 Fe4 -114.1(6) . . . . ? C12 Mo3 O8 Fe4 -104.0(6) . . . . ? O9 Fe4 O8 Mo3 33.4(6) . . . . ? N15 Fe4 O8 Mo3 -141.4(6) . . . . ? N16 Fe4 O8 Mo3 123.4(6) . . . . ? N13 Fe4 O8 Mo3 -89.0(10) . . . . ? N14 Fe4 O8 Mo3 -63.0(6) . . . . ? O12 Mo4 O9 Fe4 -41.2(8) . . . . ? O10 Mo4 O9 Fe4 70.7(7) . . . . ? C16 Mo4 O9 Fe4 -136.8(7) . . . . ? C20 Mo4 O9 Fe4 -166.6(7) . . . . ? C17 Mo4 O9 Fe4 -140.2(6) . . . . ? C19 Mo4 O9 Fe4 164.5(7) . . . . ? C18 Mo4 O9 Fe4 169.1(6) . . . . ? O8 Fe4 O9 Mo4 -95.3(7) . . . . ? N15 Fe4 O9 Mo4 53.9(13) . . . . ? N16 Fe4 O9 Mo4 149.2(7) . . . . ? N13 Fe4 O9 Mo4 74.7(7) . . . . ? N14 Fe4 O9 Mo4 -1.3(8) . . . . ? O12 Mo4 O10 Fe3 88.7(5) . . . . ? O9 Mo4 O10 Fe3 -22.5(6) . . . . ? C16 Mo4 O10 Fe3 -159.6(4) . . . . ? C20 Mo4 O10 Fe3 -119.3(5) . . . . ? C17 Mo4 O10 Fe3 178.9(5) . . . . ? C19 Mo4 O10 Fe3 -128.0(5) . . . . ? C18 Mo4 O10 Fe3 -161.5(5) . . . . ? O7 Fe3 O10 Mo4 44.6(5) . . . . ? N10 Fe3 O10 Mo4 134.7(5) . . . . ? N11 Fe3 O10 Mo4 -130.3(5) . . . . ? N12 Fe3 O10 Mo4 -50.2(5) . . . . ? O11 Mo3 C11 C12 -170.3(3) . . . . ? O7 Mo3 C11 C12 -63.7(3) . . . . ? O8 Mo3 C11 C12 70.1(4) . . . . ? C14 Mo3 C11 C12 77.4(3) . . . . ? C15 Mo3 C11 C12 113.9(5) . . . . ? C13 Mo3 C11 C12 36.3(3) . . . . ? O11 Mo3 C11 C15 75.8(3) . . . . ? O7 Mo3 C11 C15 -177.7(3) . . . . ? O8 Mo3 C11 C15 -43.8(4) . . . . ? C14 Mo3 C11 C15 -36.5(3) . . . . ? C13 Mo3 C11 C15 -77.6(3) . . . . ? C12 Mo3 C11 C15 -113.9(5) . . . . ? O11 Mo3 C11 C31 -46.2(5) . . . . ? O7 Mo3 C11 C31 60.3(5) . . . . ? O8 Mo3 C11 C31 -165.9(4) . . . . ? C14 Mo3 C11 C31 -158.5(5) . . . . ? C15 Mo3 C11 C31 -122.1(6) . . . . ? C13 Mo3 C11 C31 160.3(5) . . . . ? C12 Mo3 C11 C31 124.0(6) . . . . ? C15 C11 C12 C13 3.2(6) . . . . ? C31 C11 C12 C13 178.0(5) . . . . ? Mo3 C11 C12 C13 -64.0(4) . . . . ? C15 C11 C12 C32 -179.9(5) . . . . ? C31 C11 C12 C32 -5.1(9) . . . . ? Mo3 C11 C12 C32 112.9(5) . . . . ? C15 C11 C12 Mo3 67.2(4) . . . . ? C31 C11 C12 Mo3 -118.0(6) . . . . ? O11 Mo3 C12 C13 129.0(3) . . . . ? O7 Mo3 C12 C13 -125.2(3) . . . . ? O8 Mo3 C12 C13 -18.4(4) . . . . ? C11 Mo3 C12 C13 116.8(4) . . . . ? C14 Mo3 C12 C13 38.0(3) . . . . ? C15 Mo3 C12 C13 78.6(3) . . . . ? O11 Mo3 C12 C11 12.2(4) . . . . ? O7 Mo3 C12 C11 118.0(3) . . . . ? O8 Mo3 C12 C11 -135.1(3) . . . . ? C14 Mo3 C12 C11 -78.8(3) . . . . ? C15 Mo3 C12 C11 -38.2(3) . . . . ? C13 Mo3 C12 C11 -116.8(4) . . . . ? O11 Mo3 C12 C32 -109.2(4) . . . . ? O7 Mo3 C12 C32 -3.4(4) . . . . ? O8 Mo3 C12 C32 103.4(4) . . . . ? C11 Mo3 C12 C32 -121.4(6) . . . . ? C14 Mo3 C12 C32 159.8(5) . . . . ? C15 Mo3 C12 C32 -159.6(5) . . . . ? C13 Mo3 C12 C32 121.8(6) . . . . ? C11 C12 C13 C14 -2.4(6) . . . . ? C32 C12 C13 C14 -179.3(5) . . . . ? Mo3 C12 C13 C14 -65.5(4) . . . . ? C11 C12 C13 C33 177.5(5) . . . . ? C32 C12 C13 C33 0.6(9) . . . . ? Mo3 C12 C13 C33 114.5(5) . . . . ? C11 C12 C13 Mo3 63.0(4) . . . . ? C32 C12 C13 Mo3 -113.8(5) . . . . ? O11 Mo3 C13 C12 -82.4(4) . . . . ? O7 Mo3 C13 C12 57.2(3) . . . . ? O8 Mo3 C13 C12 164.2(3) . . . . ? C11 Mo3 C13 C12 -36.9(3) . . . . ? C14 Mo3 C13 C12 -114.5(5) . . . . ? C15 Mo3 C13 C12 -78.2(3) . . . . ? O11 Mo3 C13 C14 32.2(5) . . . . ? O7 Mo3 C13 C14 171.7(3) . . . . ? O8 Mo3 C13 C14 -81.2(4) . . . . ? C11 Mo3 C13 C14 77.7(4) . . . . ? C15 Mo3 C13 C14 36.4(3) . . . . ? C12 Mo3 C13 C14 114.5(5) . . . . ? O11 Mo3 C13 C33 153.4(4) . . . . ? O7 Mo3 C13 C33 -67.1(5) . . . . ? O8 Mo3 C13 C33 40.0(4) . . . . ? C11 Mo3 C13 C33 -161.2(5) . . . . ? C14 Mo3 C13 C33 121.2(6) . . . . ? C15 Mo3 C13 C33 157.5(5) . . . . ? C12 Mo3 C13 C33 -124.3(5) . . . . ? C12 C13 C14 C15 0.7(6) . . . . ? C33 C13 C14 C15 -179.3(5) . . . . ? Mo3 C13 C14 C15 -65.2(4) . . . . ? C12 C13 C14 C34 -179.8(5) . . . . ? C33 C13 C14 C34 0.3(9) . . . . ? Mo3 C13 C14 C34 114.3(6) . . . . ? C12 C13 C14 Mo3 65.9(4) . . . . ? C33 C13 C14 Mo3 -114.0(5) . . . . ? O11 Mo3 C14 C15 -42.8(4) . . . . ? O7 Mo3 C14 C15 104.3(4) . . . . ? O8 Mo3 C14 C15 -147.4(3) . . . . ? C11 Mo3 C14 C15 37.4(3) . . . . ? C13 Mo3 C14 C15 116.3(5) . . . . ? C12 Mo3 C14 C15 78.9(4) . . . . ? O11 Mo3 C14 C13 -159.2(3) . . . . ? O7 Mo3 C14 C13 -12.1(5) . . . . ? O8 Mo3 C14 C13 96.3(4) . . . . ? C11 Mo3 C14 C13 -79.0(4) . . . . ? C15 Mo3 C14 C13 -116.3(5) . . . . ? C12 Mo3 C14 C13 -37.5(3) . . . . ? O11 Mo3 C14 C34 80.5(4) . . . . ? O7 Mo3 C14 C34 -132.4(4) . . . . ? O8 Mo3 C14 C34 -24.0(4) . . . . ? C11 Mo3 C14 C34 160.7(5) . . . . ? C15 Mo3 C14 C34 123.4(5) . . . . ? C13 Mo3 C14 C34 -120.3(6) . . . . ? C12 Mo3 C14 C34 -157.8(5) . . . . ? C13 C14 C15 C11 1.3(6) . . . . ? C34 C14 C15 C11 -178.2(6) . . . . ? Mo3 C14 C15 C11 -63.7(4) . . . . ? C13 C14 C15 C35 179.3(6) . . . . ? C34 C14 C15 C35 -0.2(10) . . . . ? Mo3 C14 C15 C35 114.3(6) . . . . ? C13 C14 C15 Mo3 65.0(4) . . . . ? C34 C14 C15 Mo3 -114.5(6) . . . . ? C12 C11 C15 C14 -2.8(6) . . . . ? C31 C11 C15 C14 -177.7(5) . . . . ? Mo3 C11 C15 C14 64.6(4) . . . . ? C12 C11 C15 C35 179.1(5) . . . . ? C31 C11 C15 C35 4.3(9) . . . . ? Mo3 C11 C15 C35 -113.4(6) . . . . ? C12 C11 C15 Mo3 -67.4(4) . . . . ? C31 C11 C15 Mo3 117.7(6) . . . . ? O11 Mo3 C15 C14 140.2(4) . . . . ? O7 Mo3 C15 C14 -112.8(4) . . . . ? O8 Mo3 C15 C14 35.2(4) . . . . ? C11 Mo3 C15 C14 -116.0(4) . . . . ? C13 Mo3 C15 C14 -37.1(3) . . . . ? C12 Mo3 C15 C14 -77.9(3) . . . . ? O11 Mo3 C15 C11 -103.7(3) . . . . ? O7 Mo3 C15 C11 3.3(4) . . . . ? O8 Mo3 C15 C11 151.2(3) . . . . ? C14 Mo3 C15 C11 116.0(5) . . . . ? C13 Mo3 C15 C11 78.9(3) . . . . ? C12 Mo3 C15 C11 38.2(3) . . . . ? O11 Mo3 C15 C35 15.6(5) . . . . ? O7 Mo3 C15 C35 122.6(5) . . . . ? O8 Mo3 C15 C35 -89.5(5) . . . . ? C11 Mo3 C15 C35 119.3(6) . . . . ? C14 Mo3 C15 C35 -124.7(7) . . . . ? C13 Mo3 C15 C35 -161.8(6) . . . . ? C12 Mo3 C15 C35 157.5(6) . . . . ? O12 Mo4 C16 C20 -167.5(3) . . . . ? O9 Mo4 C16 C20 -62.0(4) . . . . ? O10 Mo4 C16 C20 76.0(4) . . . . ? C17 Mo4 C16 C20 114.0(5) . . . . ? C19 Mo4 C16 C20 37.3(3) . . . . ? C18 Mo4 C16 C20 78.3(3) . . . . ? O12 Mo4 C16 C17 78.5(3) . . . . ? O9 Mo4 C16 C17 -175.9(3) . . . . ? O10 Mo4 C16 C17 -38.0(5) . . . . ? C20 Mo4 C16 C17 -114.0(5) . . . . ? C19 Mo4 C16 C17 -76.7(4) . . . . ? C18 Mo4 C16 C17 -35.7(3) . . . . ? O12 Mo4 C16 C36 -43.7(5) . . . . ? O9 Mo4 C16 C36 61.9(5) . . . . ? O10 Mo4 C16 C36 -160.1(4) . . . . ? C20 Mo4 C16 C36 123.9(6) . . . . ? C17 Mo4 C16 C36 -122.1(6) . . . . ? C19 Mo4 C16 C36 161.2(5) . . . . ? C18 Mo4 C16 C36 -157.8(5) . . . . ? C20 C16 C17 C18 -1.2(5) . . . . ? C36 C16 C17 C18 -174.0(5) . . . . ? Mo4 C16 C17 C18 65.8(3) . . . . ? C20 C16 C17 C37 178.7(4) . . . . ? C36 C16 C17 C37 5.9(8) . . . . ? Mo4 C16 C17 C37 -114.4(5) . . . . ? C20 C16 C17 Mo4 -66.9(3) . . . . ? C36 C16 C17 Mo4 120.2(5) . . . . ? O12 Mo4 C17 C18 142.4(3) . . . . ? O9 Mo4 C17 C18 -111.1(4) . . . . ? O10 Mo4 C17 C18 37.7(4) . . . . ? C16 Mo4 C17 C18 -117.0(5) . . . . ? C20 Mo4 C17 C18 -78.8(4) . . . . ? C19 Mo4 C17 C18 -37.4(3) . . . . ? O12 Mo4 C17 C16 -100.6(3) . . . . ? O9 Mo4 C17 C16 5.9(5) . . . . ? O10 Mo4 C17 C16 154.6(3) . . . . ? C20 Mo4 C17 C16 38.2(3) . . . . ? C19 Mo4 C17 C16 79.5(4) . . . . ? C18 Mo4 C17 C16 117.0(5) . . . . ? O12 Mo4 C17 C37 17.5(5) . . . . ? O9 Mo4 C17 C37 124.0(5) . . . . ? O10 Mo4 C17 C37 -87.3(5) . . . . ? C16 Mo4 C17 C37 118.1(6) . . . . ? C20 Mo4 C17 C37 156.2(5) . . . . ? C19 Mo4 C17 C37 -162.4(5) . . . . ? C18 Mo4 C17 C37 -124.9(6) . . . . ? C16 C17 C18 C19 0.1(5) . . . . ? C37 C17 C18 C19 -179.8(5) . . . . ? Mo4 C17 C18 C19 63.3(3) . . . . ? C16 C17 C18 C38 -179.5(5) . . . . ? C37 C17 C18 C38 0.6(8) . . . . ? Mo4 C17 C18 C38 -116.3(5) . . . . ? C16 C17 C18 Mo4 -63.2(3) . . . . ? C37 C17 C18 Mo4 116.9(5) . . . . ? O12 Mo4 C18 C17 -40.6(4) . . . . ? O9 Mo4 C18 C17 107.9(4) . . . . ? O10 Mo4 C18 C17 -144.4(3) . . . . ? C16 Mo4 C18 C17 37.1(3) . . . . ? C20 Mo4 C18 C17 78.5(3) . . . . ? C19 Mo4 C18 C17 115.9(5) . . . . ? O12 Mo4 C18 C19 -156.5(3) . . . . ? O9 Mo4 C18 C19 -8.0(5) . . . . ? O10 Mo4 C18 C19 99.6(3) . . . . ? C16 Mo4 C18 C19 -78.9(4) . . . . ? C20 Mo4 C18 C19 -37.5(3) . . . . ? C17 Mo4 C18 C19 -115.9(5) . . . . ? O12 Mo4 C18 C38 83.6(5) . . . . ? O9 Mo4 C18 C38 -127.9(4) . . . . ? O10 Mo4 C18 C38 -20.3(5) . . . . ? C16 Mo4 C18 C38 161.2(5) . . . . ? C20 Mo4 C18 C38 -157.4(5) . . . . ? C17 Mo4 C18 C38 124.2(6) . . . . ? C19 Mo4 C18 C38 -119.9(6) . . . . ? C17 C18 C19 C20 1.0(5) . . . . ? C38 C18 C19 C20 -179.3(5) . . . . ? Mo4 C18 C19 C20 64.6(3) . . . . ? C17 C18 C19 C39 -179.6(5) . . . . ? C38 C18 C19 C39 0.1(8) . . . . ? Mo4 C18 C19 C39 -116.1(5) . . . . ? C17 C18 C19 Mo4 -63.5(3) . . . . ? C38 C18 C19 Mo4 116.1(5) . . . . ? O12 Mo4 C19 C20 -79.2(4) . . . . ? O9 Mo4 C19 C20 59.2(3) . . . . ? O10 Mo4 C19 C20 166.8(3) . . . . ? C16 Mo4 C19 C20 -37.4(3) . . . . ? C17 Mo4 C19 C20 -79.0(3) . . . . ? C18 Mo4 C19 C20 -115.3(5) . . . . ? O12 Mo4 C19 C18 36.2(5) . . . . ? O9 Mo4 C19 C18 174.5(3) . . . . ? O10 Mo4 C19 C18 -77.8(3) . . . . ? C16 Mo4 C19 C18 77.9(3) . . . . ? C20 Mo4 C19 C18 115.3(5) . . . . ? C17 Mo4 C19 C18 36.3(3) . . . . ? O12 Mo4 C19 C39 157.8(4) . . . . ? O9 Mo4 C19 C39 -63.8(5) . . . . ? O10 Mo4 C19 C39 43.8(4) . . . . ? C16 Mo4 C19 C39 -160.5(5) . . . . ? C20 Mo4 C19 C39 -123.0(6) . . . . ? C17 Mo4 C19 C39 158.0(5) . . . . ? C18 Mo4 C19 C39 121.6(6) . . . . ? C17 C16 C20 C19 1.8(5) . . . . ? C36 C16 C20 C19 174.4(5) . . . . ? Mo4 C16 C20 C19 -65.8(3) . . . . ? C17 C16 C20 C40 -176.9(5) . . . . ? C36 C16 C20 C40 -4.3(8) . . . . ? Mo4 C16 C20 C40 115.5(5) . . . . ? C17 C16 C20 Mo4 67.6(3) . . . . ? C36 C16 C20 Mo4 -119.8(5) . . . . ? C18 C19 C20 C16 -1.8(5) . . . . ? C39 C19 C20 C16 178.9(5) . . . . ? Mo4 C19 C20 C16 64.4(3) . . . . ? C18 C19 C20 C40 177.1(4) . . . . ? C39 C19 C20 C40 -2.3(8) . . . . ? Mo4 C19 C20 C40 -116.8(5) . . . . ? C18 C19 C20 Mo4 -66.2(3) . . . . ? C39 C19 C20 Mo4 114.5(5) . . . . ? O12 Mo4 C20 C16 15.3(4) . . . . ? O9 Mo4 C20 C16 120.7(3) . . . . ? O10 Mo4 C20 C16 -131.1(3) . . . . ? C17 Mo4 C20 C16 -38.2(3) . . . . ? C19 Mo4 C20 C16 -115.5(5) . . . . ? C18 Mo4 C20 C16 -78.1(3) . . . . ? O12 Mo4 C20 C19 130.8(3) . . . . ? O9 Mo4 C20 C19 -123.8(3) . . . . ? O10 Mo4 C20 C19 -15.6(4) . . . . ? C16 Mo4 C20 C19 115.5(5) . . . . ? C17 Mo4 C20 C19 77.3(3) . . . . ? C18 Mo4 C20 C19 37.3(3) . . . . ? O12 Mo4 C20 C40 -108.6(5) . . . . ? O9 Mo4 C20 C40 -3.2(5) . . . . ? O10 Mo4 C20 C40 104.9(5) . . . . ? C16 Mo4 C20 C40 -123.9(6) . . . . ? C17 Mo4 C20 C40 -162.2(6) . . . . ? C19 Mo4 C20 C40 120.6(6) . . . . ? C18 Mo4 C20 C40 157.9(6) . . . . ? C49 N9 C47 C59 159.7(4) . . . . ? C48 N9 C47 C59 -75.2(5) . . . . ? Fe3 N9 C47 C59 44.2(5) . . . . ? C47 N9 C48 C60 141.9(4) . . . . ? C49 N9 C48 C60 -92.7(5) . . . . ? Fe3 N9 C48 C60 24.1(5) . . . . ? C47 N9 C49 C61 -163.9(4) . . . . ? C48 N9 C49 C61 71.2(5) . . . . ? Fe3 N9 C49 C61 -47.7(4) . . . . ? C52 N13 C50 C62 -163.4(5) . . . . ? C51 N13 C50 C62 72.8(6) . . . . ? Fe4 N13 C50 C62 -46.7(5) . . . . ? C50 N13 C51 C63 -91.0(6) . . . . ? C52 N13 C51 C63 143.4(5) . . . . ? Fe4 N13 C51 C63 26.5(5) . . . . ? C50 N13 C52 C64 162.3(5) . . . . ? C51 N13 C52 C64 -73.1(6) . . . . ? Fe4 N13 C52 C64 45.6(5) . . . . ? C92 N10 C59 C89 0.8(8) . . . . ? Fe3 N10 C59 C89 -179.8(4) . . . . ? C92 N10 C59 C47 -177.8(5) . . . . ? Fe3 N10 C59 C47 1.6(6) . . . . ? N9 C47 C59 N10 -31.9(6) . . . . ? N9 C47 C59 C89 149.6(5) . . . . ? C96 N11 C60 C93 2.0(8) . . . . ? Fe3 N11 C60 C93 -158.2(4) . . . . ? C96 N11 C60 C48 -174.3(5) . . . . ? Fe3 N11 C60 C48 25.4(6) . . . . ? N9 C48 C60 N11 -34.1(7) . . . . ? N9 C48 C60 C93 149.5(5) . . . . ? C100 N12 C61 C97 0.5(7) . . . . ? Fe3 N12 C61 C97 160.1(4) . . . . ? C100 N12 C61 C49 -179.0(4) . . . . ? Fe3 N12 C61 C49 -19.5(5) . . . . ? N9 C49 C61 N12 46.5(6) . . . . ? N9 C49 C61 C97 -133.0(5) . . . . ? C104 N14 C62 C101 -0.1(8) . . . . ? Fe4 N14 C62 C101 157.6(5) . . . . ? C104 N14 C62 C50 -177.7(5) . . . . ? Fe4 N14 C62 C50 -20.1(6) . . . . ? N13 C50 C62 N14 46.0(7) . . . . ? N13 C50 C62 C101 -131.6(6) . . . . ? C108 N15 C63 C105 1.2(8) . . . . ? Fe4 N15 C63 C105 -160.1(4) . . . . ? C108 N15 C63 C51 -175.7(5) . . . . ? Fe4 N15 C63 C51 23.0(6) . . . . ? N13 C51 C63 N15 -34.0(7) . . . . ? N13 C51 C63 C105 149.0(5) . . . . ? C112 N16 C64 C109 -0.8(8) . . . . ? Fe4 N16 C64 C109 178.7(4) . . . . ? C112 N16 C64 C52 -179.4(5) . . . . ? Fe4 N16 C64 C52 0.2(6) . . . . ? N13 C52 C64 N16 -31.6(7) . . . . ? N13 C52 C64 C109 149.8(6) . . . . ? N10 C59 C89 C90 -1.0(9) . . . . ? C47 C59 C89 C90 177.5(5) . . . . ? C59 C89 C90 C91 -0.3(9) . . . . ? C89 C90 C91 C92 1.7(9) . . . . ? C59 N10 C92 C91 0.8(8) . . . . ? Fe3 N10 C92 C91 -178.6(4) . . . . ? C90 C91 C92 N10 -2.0(9) . . . . ? N11 C60 C93 C94 -2.3(9) . . . . ? C48 C60 C93 C94 173.8(5) . . . . ? C60 C93 C94 C95 0.2(9) . . . . ? C93 C94 C95 C96 2.2(9) . . . . ? C60 N11 C96 C95 0.5(8) . . . . ? Fe3 N11 C96 C95 158.5(4) . . . . ? C94 C95 C96 N11 -2.5(9) . . . . ? N12 C61 C97 C98 -0.8(8) . . . . ? C49 C61 C97 C98 178.7(5) . . . . ? C61 C97 C98 C99 0.7(9) . . . . ? C97 C98 C99 C100 -0.2(9) . . . . ? C61 N12 C100 C99 0.0(8) . . . . ? Fe3 N12 C100 C99 -157.1(4) . . . . ? C98 C99 C100 N12 -0.2(8) . . . . ? N14 C62 C101 C102 0.5(9) . . . . ? C50 C62 C101 C102 177.9(6) . . . . ? C62 C101 C102 C103 -0.8(10) . . . . ? C101 C102 C103 C104 0.6(10) . . . . ? C62 N14 C104 C103 -0.1(8) . . . . ? Fe4 N14 C104 C103 -155.6(5) . . . . ? C102 C103 C104 N14 -0.2(9) . . . . ? N15 C63 C105 C106 -2.8(9) . . . . ? C51 C63 C105 C106 174.0(5) . . . . ? C63 C105 C106 C107 2.0(9) . . . . ? C105 C106 C107 C108 0.3(9) . . . . ? C63 N15 C108 C107 1.2(8) . . . . ? Fe4 N15 C108 C107 160.6(4) . . . . ? C106 C107 C108 N15 -1.9(9) . . . . ? N16 C64 C109 C110 -1.4(9) . . . . ? C52 C64 C109 C110 177.1(6) . . . . ? C64 C109 C110 C111 2.2(9) . . . . ? C109 C110 C111 C112 -0.8(9) . . . . ? C64 N16 C112 C111 2.3(8) . . . . ? Fe4 N16 C112 C111 -177.2(4) . . . . ? C110 C111 C112 N16 -1.5(9) . . . . ? O201 S200 C200 F201 179.3(5) . . . . ? O202 S200 C200 F201 58.7(5) . . . . ? O203 S200 C200 F201 -61.0(5) . . . . ? O201 S200 C200 F202 -60.4(5) . . . . ? O202 S200 C200 F202 179.0(5) . . . . ? O203 S200 C200 F202 59.2(5) . . . . ? O201 S200 C200 F203 58.5(6) . . . . ? O202 S200 C200 F203 -62.1(6) . . . . ? O203 S200 C200 F203 178.1(5) . . . . ? O301 S300 C300 F302 -177.8(4) . . . . ? O302 S300 C300 F302 -56.8(5) . . . . ? O303 S300 C300 F302 62.9(5) . . . . ? O301 S300 C300 F303 61.5(5) . . . . ? O302 S300 C300 F303 -177.5(4) . . . . ? O303 S300 C300 F303 -57.8(5) . . . . ? O301 S300 C300 F301 -58.4(4) . . . . ? O302 S300 C300 F301 62.5(4) . . . . ? O303 S300 C300 F301 -177.8(4) . . . . ? O402 S400 C400 F402 171.9(10) . . . . ? O401 S400 C400 F402 -82.4(10) . . . . ? O403 S400 C400 F402 27.2(10) . . . . ? O402 S400 C400 F401 -54.0(9) . . . . ? O401 S400 C400 F401 51.7(8) . . . . ? O403 S400 C400 F401 161.3(7) . . . . ? O402 S400 C400 F403 61.2(8) . . . . ? O401 S400 C400 F403 166.9(7) . . . . ? O403 S400 C400 F403 -83.5(7) . . . . ? C410 O412 S410 O413 97.9(9) . . . . ? C410 O412 S410 O411 -111.4(18) . . . . ? O413 S410 C410 F412 -177.2(11) . . . . ? O411 S410 C410 F412 47.7(17) . . . . ? O412 S410 C410 F412 -76.3(12) . . . . ? O413 S410 C410 F411 -56.3(12) . . . . ? O411 S410 C410 F411 168.5(15) . . . . ? O412 S410 C410 F411 44.6(12) . . . . ? O413 S410 C410 F413 62.2(12) . . . . ? O411 S410 C410 F413 -73.0(17) . . . . ? O412 S410 C410 F413 163.1(13) . . . . ? O413 S410 C410 O412 -100.9(12) . . . . ? O411 S410 C410 O412 123.9(17) . . . . ? S410 O412 C410 F412 116.0(10) . . . . ? S410 O412 C410 F411 -139.2(11) . . . . ? S410 O412 C410 F413 -36(3) . . . . ? O501 S500 C500 F502 -63.6(8) . . . . ? O503 S500 C500 F502 176.1(7) . . . . ? O502 S500 C500 F502 53.2(9) . . . . ? O501 S500 C500 F503 -179.9(8) . . . . ? O503 S500 C500 F503 59.7(8) . . . . ? O502 S500 C500 F503 -63.2(9) . . . . ? O501 S500 C500 F501 53.8(8) . . . . ? O503 S500 C500 F501 -66.6(8) . . . . ? O502 S500 C500 F501 170.5(9) . . . . ? O512 S510 C510 F512 -61.1(9) . . . . ? O511 S510 C510 F512 176.0(7) . . . . ? O513 S510 C510 F512 57.5(7) . . . . ? O512 S510 C510 F513 -175.7(8) . . . . ? O511 S510 C510 F513 61.4(7) . . . . ? O513 S510 C510 F513 -57.2(7) . . . . ? O512 S510 C510 F511 61.1(9) . . . . ? O511 S510 C510 F511 -61.8(8) . . . . ? O513 S510 C510 F511 179.7(7) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 936995' ####################################################################### # # 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_jf124_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H33 Mo N4 O3 Zn, 0.5(C6 H9 N3), C F3 O3 S, 0.5(C2 H3 N)' _chemical_formula_sum 'C33 H39 F3 Mo N6 O6 S Zn' _chemical_formula_weight 866.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F .0171 .0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 .6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn .2839 1.4301 '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 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 19.2094(6) _cell_length_b 14.0319(3) _cell_length_c 14.4470(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.646(2) _cell_angle_gamma 90.00 _cell_volume 3730.92(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 64644 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 29.54 _exptl_crystal_description 'very thin plate' _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.542 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1768 _exptl_absorpt_coefficient_mu 1.100 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6673 _exptl_absorpt_correction_T_max 0.9369 _exptl_absorpt_process_details 'PLATON, 1990' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'long fine focus sealed X-ray tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_collimation '0.5 mm diameter monocapillary' _diffrn_measurement_device 'Stoe IPDS-2t diffractometer' _diffrn_measurement_method '\w-rotation,\w-incr.=1\%,319 exposures' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 65943 _diffrn_reflns_av_R_equivalents 0.1160 _diffrn_reflns_av_sigmaI/netI 0.0488 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6568 _reflns_number_gt 5408 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-RED (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON, 1990' _computing_publication_material 'PLATON, 1990' _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^)+(0.0954P)^2^+28.4859P] 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 0.0038(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6568 _refine_ls_number_parameters 453 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1027 _refine_ls_R_factor_gt 0.0863 _refine_ls_wR_factor_ref 0.2174 _refine_ls_wR_factor_gt 0.2070 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.010 _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 0.44564(4) 0.24739(4) 0.18323(5) 0.0343(3) Uani 1 1 d . . . Zn1 Zn 0.28856(5) 0.39727(6) 0.14564(7) 0.0372(3) Uani 1 1 d . . . O1 O 0.3771(3) 0.3236(4) 0.2054(4) 0.0380(12) Uani 1 1 d . . . O2 O 0.5053(3) 0.3203(4) 0.1475(4) 0.0414(14) Uani 1 1 d . . . O3 O 0.4031(4) 0.1803(4) 0.0827(4) 0.0484(15) Uani 1 1 d . . . N1 N 0.3210(4) 0.4860(4) 0.0513(5) 0.0360(15) Uani 1 1 d . . . N2 N 0.1895(4) 0.4867(6) 0.0883(5) 0.0485(18) Uani 1 1 d . . . N3 N 0.2119(4) 0.2951(6) 0.0878(6) 0.0485(18) Uani 1 1 d . . . N4 N 0.2769(4) 0.4634(5) 0.2689(5) 0.0440(17) Uani 1 1 d . . . C1 C 0.2675(5) 0.5387(6) -0.0094(6) 0.043(2) Uani 1 1 d . . . C2 C 0.1906(5) 0.5167(7) -0.0097(7) 0.051(2) Uani 1 1 d . . . H13 H 0.1604 0.5727 -0.0293 0.061 Uiso 1 1 calc R . . H14 H 0.1711 0.4661 -0.0556 0.061 Uiso 1 1 calc R . . C3 C 0.1284(5) 0.4231(8) 0.0843(8) 0.062(3) Uani 1 1 d . . . H5 H 0.0863 0.4450 0.0340 0.074 Uiso 1 1 calc R . . H6 H 0.1167 0.4267 0.1453 0.074 Uiso 1 1 calc R . . C4 C 0.1434(6) 0.3208(8) 0.0649(7) 0.056(2) Uani 1 1 d . . . C5 C 0.2287(6) 0.2026(8) 0.0767(9) 0.068(3) Uani 1 1 d . . . H4 H 0.2772 0.1842 0.0919 0.081 Uiso 1 1 calc R . . C6 C 0.1755(8) 0.1363(9) 0.0436(12) 0.097(5) Uani 1 1 d . . . H3 H 0.1870 0.0726 0.0377 0.117 Uiso 1 1 calc R . . C7 C 0.1040(8) 0.1662(12) 0.0189(12) 0.102(5) Uani 1 1 d . . . H2 H 0.0670 0.1225 -0.0062 0.123 Uiso 1 1 calc R . . C8 C 0.0872(7) 0.2576(10) 0.0309(9) 0.077(3) Uani 1 1 d . . . H1 H 0.0391 0.2774 0.0165 0.092 Uiso 1 1 calc R . . C9 C 0.1950(5) 0.5683(7) 0.1546(7) 0.053(2) Uani 1 1 d . . . H11 H 0.1468 0.5923 0.1500 0.063 Uiso 1 1 calc R . . H12 H 0.2226 0.6191 0.1362 0.063 Uiso 1 1 calc R . . C10 C 0.2317(5) 0.5382(7) 0.2563(7) 0.051(2) Uani 1 1 d . . . C11 C 0.3145(6) 0.4359(7) 0.3592(7) 0.053(2) Uani 1 1 d . . . H10 H 0.3442 0.3825 0.3669 0.063 Uiso 1 1 calc R . . C12 C 0.3102(7) 0.4845(7) 0.4396(7) 0.065(3) Uani 1 1 d . . . H9 H 0.3374 0.4658 0.5010 0.079 Uiso 1 1 calc R . . C13 C 0.2640(8) 0.5624(8) 0.4267(8) 0.082(4) Uani 1 1 d . . . H8 H 0.2600 0.5970 0.4799 0.099 Uiso 1 1 calc R . . C14 C 0.2242(7) 0.5882(8) 0.3352(8) 0.073(3) Uani 1 1 d . . . H7 H 0.1922 0.6393 0.3264 0.087 Uiso 1 1 calc R . . C15 C 0.2833(5) 0.6071(6) -0.0693(6) 0.048(2) Uani 1 1 d . . . H18 H 0.2466 0.6446 -0.1083 0.058 Uiso 1 1 calc R . . C16 C 0.3550(5) 0.6191(6) -0.0704(6) 0.046(2) Uani 1 1 d . . . H17 H 0.3667 0.6630 -0.1118 0.055 Uiso 1 1 calc R . . C17 C 0.4082(5) 0.5648(5) -0.0091(5) 0.0341(17) Uani 1 1 d . . . H16 H 0.4565 0.5721 -0.0082 0.041 Uiso 1 1 calc R . . C18 C 0.3896(4) 0.5001(5) 0.0506(5) 0.0326(16) Uani 1 1 d . . . H15 H 0.4262 0.4644 0.0923 0.039 Uiso 1 1 calc R . . C19 C 0.5521(5) 0.1962(5) 0.3084(6) 0.0403(19) Uani 1 1 d . . . C20 C 0.5032(5) 0.2298(5) 0.3587(5) 0.0339(18) Uani 1 1 d . . . C21 C 0.4417(5) 0.1695(5) 0.3369(6) 0.0397(19) Uani 1 1 d . . . C22 C 0.4520(5) 0.0976(5) 0.2728(6) 0.0402(19) Uani 1 1 d . . . C23 C 0.5192(5) 0.1152(5) 0.2535(6) 0.040(2) Uani 1 1 d . . . C24 C 0.5502(6) 0.0561(6) 0.1886(6) 0.051(2) Uani 1 1 d . . . H19 H 0.5702 -0.0016 0.2213 0.076 Uiso 1 1 calc R . . H20 H 0.5877 0.0913 0.1720 0.076 Uiso 1 1 calc R . . H21 H 0.5125 0.0406 0.1308 0.076 Uiso 1 1 calc R . . C25 C 0.4003(6) 0.0178(5) 0.2303(6) 0.048(2) Uani 1 1 d . . . H22 H 0.4201 -0.0414 0.2594 0.072 Uiso 1 1 calc R . . H23 H 0.3934 0.0148 0.1619 0.072 Uiso 1 1 calc R . . H24 H 0.3544 0.0293 0.2425 0.072 Uiso 1 1 calc R . . C26 C 0.3770(5) 0.1800(6) 0.3744(6) 0.049(2) Uani 1 1 d . . . H25 H 0.3420 0.2212 0.3324 0.074 Uiso 1 1 calc R . . H26 H 0.3921 0.2070 0.4381 0.074 Uiso 1 1 calc R . . H27 H 0.3556 0.1186 0.3769 0.074 Uiso 1 1 calc R . . C27 C 0.5171(6) 0.3119(5) 0.4276(6) 0.046(2) Uani 1 1 d . . . H28 H 0.5366 0.2886 0.4924 0.069 Uiso 1 1 calc R . . H29 H 0.4724 0.3449 0.4222 0.069 Uiso 1 1 calc R . . H30 H 0.5513 0.3547 0.4125 0.069 Uiso 1 1 calc R . . C28 C 0.6249(5) 0.2356(6) 0.3161(7) 0.049(2) Uani 1 1 d . . . H31 H 0.6216 0.3035 0.3082 0.074 Uiso 1 1 calc R . . H32 H 0.6432 0.2083 0.2667 0.074 Uiso 1 1 calc R . . H33 H 0.6573 0.2205 0.3784 0.074 Uiso 1 1 calc R . . S1 S 0.13247(16) 0.8171(2) 0.0505(3) 0.0775(9) Uani 1 1 d . . . F1 F 0.2169(5) 0.7900(5) 0.2212(5) 0.089(2) Uani 1 1 d . . . F2 F 0.2420(4) 0.9187(5) 0.1520(5) 0.0783(18) Uani 1 1 d . . . F3 F 0.1532(6) 0.9162(7) 0.2105(7) 0.122(3) Uani 1 1 d . . . O4 O 0.0808(5) 0.7600(8) 0.0814(10) 0.116(4) Uani 1 1 d . . . O5 O 0.1856(4) 0.7651(5) 0.0129(6) 0.0654(19) Uani 1 1 d . . . O6 O 0.1017(5) 0.9057(7) 0.0003(8) 0.105(3) Uani 1 1 d . . . C29 C 0.1899(6) 0.8622(8) 0.1552(9) 0.064(3) Uani 1 1 d . . . N41 N 0.0197(18) 1.013(2) 0.351(2) 0.140(4) Uiso 0.50 1 d PD A 1 C41 C 0.000(2) 0.988(3) 0.268(2) 0.140(4) Uiso 0.50 1 d PD A 1 C42 C -0.018(2) 0.976(3) 0.161(2) 0.140(4) Uiso 0.50 1 d PD A 1 H42A H -0.0520 1.0246 0.1304 0.210 Uiso 0.50 1 calc PR A 1 H42B H -0.0394 0.9145 0.1435 0.210 Uiso 0.50 1 calc PR A 1 H42C H 0.0253 0.9818 0.1415 0.210 Uiso 0.50 1 calc PR A 1 N51 N -0.0758(19) 0.820(2) 0.241(2) 0.140(4) Uiso 0.50 1 d PD B 2 C51 C -0.075(3) 0.735(2) 0.235(3) 0.140(4) Uiso 0.50 1 d PD B 2 C52 C -0.068(2) 0.635(2) 0.205(3) 0.140(4) Uiso 0.50 1 d PD B 2 H52A H -0.1116 0.6158 0.1571 0.210 Uiso 0.50 1 calc PR B 2 H52B H -0.0596 0.5938 0.2601 0.210 Uiso 0.50 1 calc PR B 2 H52C H -0.0276 0.6302 0.1783 0.210 Uiso 0.50 1 calc PR B 2 N61 N 0.0096(18) 0.838(2) 0.275(3) 0.140(4) Uiso 0.50 1 d PD C 3 C61 C -0.002(2) 0.749(2) 0.271(3) 0.140(4) Uiso 0.50 1 d PD C 3 C62 C 0.016(2) 0.647(2) 0.257(3) 0.140(4) Uiso 0.50 1 d PD C 3 H62A H -0.0027 0.6307 0.1897 0.210 Uiso 0.50 1 calc PR C 3 H62B H -0.0047 0.6064 0.2948 0.210 Uiso 0.50 1 calc PR C 3 H62C H 0.0681 0.6396 0.2763 0.210 Uiso 0.50 1 calc PR C 3 N71 N -0.145(2) 0.745(2) 0.191(3) 0.140(4) Uiso 0.50 1 d PD D 4 C71 C -0.176(2) 0.676(2) 0.202(3) 0.140(4) Uiso 0.50 1 d PD D 4 C72 C -0.190(2) 0.571(2) 0.220(3) 0.140(4) Uiso 0.50 1 d PD D 4 H72A H -0.1558 0.5317 0.2002 0.210 Uiso 0.50 1 calc PR D 4 H72B H -0.2383 0.5543 0.1840 0.210 Uiso 0.50 1 calc PR D 4 H72C H -0.1838 0.5617 0.2878 0.210 Uiso 0.50 1 calc PR D 4 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 0.0629(5) 0.0211(3) 0.0281(4) 0.0029(2) 0.0279(3) 0.0011(3) Zn1 0.0509(6) 0.0330(5) 0.0363(5) 0.0044(4) 0.0263(4) -0.0009(4) O1 0.059(3) 0.030(3) 0.032(3) 0.003(2) 0.023(3) -0.002(2) O2 0.067(4) 0.030(3) 0.040(3) 0.012(2) 0.036(3) 0.009(3) O3 0.089(5) 0.033(3) 0.029(3) 0.002(2) 0.026(3) -0.003(3) N1 0.049(4) 0.031(3) 0.035(3) 0.006(3) 0.023(3) 0.002(3) N2 0.055(4) 0.056(5) 0.047(4) 0.010(4) 0.033(4) 0.005(4) N3 0.050(5) 0.053(5) 0.046(4) 0.006(4) 0.021(4) -0.001(4) N4 0.064(5) 0.040(4) 0.039(4) 0.007(3) 0.033(4) 0.001(3) C1 0.056(5) 0.047(5) 0.037(4) 0.004(4) 0.029(4) 0.005(4) C2 0.045(5) 0.066(6) 0.045(5) 0.012(4) 0.019(4) 0.006(4) C3 0.052(6) 0.078(7) 0.066(7) 0.017(5) 0.034(5) -0.005(5) C4 0.065(6) 0.066(6) 0.040(5) 0.006(4) 0.020(4) -0.016(5) C5 0.063(7) 0.048(6) 0.079(8) -0.003(5) -0.001(6) -0.007(5) C6 0.088(10) 0.048(7) 0.137(13) -0.005(7) 0.001(9) -0.018(6) C7 0.074(9) 0.096(11) 0.117(12) -0.023(9) -0.003(8) -0.040(8) C8 0.064(7) 0.086(9) 0.073(8) -0.009(7) 0.006(6) -0.021(6) C9 0.060(6) 0.049(5) 0.062(6) 0.009(4) 0.040(5) 0.014(4) C10 0.070(6) 0.048(5) 0.048(5) 0.015(4) 0.039(5) 0.010(4) C11 0.085(7) 0.040(5) 0.044(5) 0.006(4) 0.036(5) -0.003(5) C12 0.121(9) 0.048(6) 0.040(5) 0.008(4) 0.043(6) 0.015(6) C13 0.150(12) 0.061(7) 0.056(7) 0.008(5) 0.061(8) 0.023(7) C14 0.117(10) 0.050(6) 0.073(8) 0.010(5) 0.063(7) 0.025(6) C15 0.069(6) 0.046(5) 0.039(5) 0.016(4) 0.032(4) 0.015(4) C16 0.076(6) 0.036(4) 0.040(5) 0.008(4) 0.038(4) 0.004(4) C17 0.057(5) 0.023(3) 0.033(4) 0.003(3) 0.030(4) 0.003(3) C18 0.052(5) 0.024(3) 0.027(4) -0.006(3) 0.019(3) 0.004(3) C19 0.064(5) 0.028(4) 0.034(4) 0.009(3) 0.022(4) 0.004(4) C20 0.066(5) 0.020(4) 0.021(4) 0.004(3) 0.021(4) 0.000(3) C21 0.076(6) 0.023(4) 0.029(4) 0.004(3) 0.029(4) 0.001(4) C22 0.080(6) 0.016(3) 0.032(4) 0.003(3) 0.027(4) -0.002(4) C23 0.082(6) 0.015(3) 0.033(4) 0.005(3) 0.032(4) 0.010(4) C24 0.092(7) 0.032(4) 0.041(5) 0.005(4) 0.041(5) 0.014(4) C25 0.094(7) 0.021(4) 0.042(5) -0.002(3) 0.037(5) -0.006(4) C26 0.084(7) 0.036(4) 0.042(5) 0.003(4) 0.042(5) -0.003(4) C27 0.087(7) 0.019(4) 0.040(5) 0.000(3) 0.033(5) -0.003(4) C28 0.071(6) 0.037(5) 0.046(5) 0.010(4) 0.024(5) 0.003(4) S1 0.0601(17) 0.076(2) 0.095(2) 0.0160(17) 0.0194(16) 0.0113(15) F1 0.148(7) 0.072(4) 0.055(4) 0.005(3) 0.040(4) 0.016(4) F2 0.097(5) 0.064(4) 0.076(4) -0.009(3) 0.029(4) -0.008(4) F3 0.153(8) 0.112(7) 0.126(7) -0.016(6) 0.079(6) 0.037(6) O4 0.058(5) 0.130(9) 0.160(11) 0.025(8) 0.033(6) -0.018(5) O5 0.083(5) 0.050(4) 0.069(5) 0.008(3) 0.030(4) 0.004(4) O6 0.084(6) 0.096(7) 0.115(8) 0.020(6) -0.003(5) 0.029(5) C29 0.049(6) 0.060(6) 0.080(8) 0.019(6) 0.016(5) 0.014(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 O2 1.723(5) . ? Mo1 O3 1.728(6) . ? Mo1 O1 1.795(5) . ? Mo1 C23 2.376(8) . ? Mo1 C19 2.419(9) . ? Mo1 C22 2.453(7) . ? Mo1 C20 2.470(7) . ? Mo1 C21 2.495(7) . ? Zn1 O1 1.966(6) . ? Zn1 N3 2.054(8) . ? Zn1 N1 2.070(6) . ? Zn1 N4 2.076(7) . ? Zn1 N2 2.231(8) . ? N1 C18 1.335(10) . ? N1 C1 1.362(11) . ? N2 C3 1.463(12) . ? N2 C9 1.476(12) . ? N2 C2 1.484(11) . ? N3 C4 1.313(13) . ? N3 C5 1.358(13) . ? N4 C10 1.342(11) . ? N4 C11 1.353(12) . ? C1 C15 1.383(11) . ? C1 C2 1.509(12) . ? C2 H13 0.9700 . ? C2 H14 0.9700 . ? C3 C4 1.506(15) . ? C3 H5 0.9700 . ? C3 H6 0.9700 . ? C4 C8 1.375(15) . ? C5 C6 1.363(15) . ? C5 H4 0.9300 . ? C6 C7 1.38(2) . ? C6 H3 0.9300 . ? C7 C8 1.347(19) . ? C7 H2 0.9300 . ? C8 H1 0.9300 . ? C9 C10 1.497(13) . ? C9 H11 0.9700 . ? C9 H12 0.9700 . ? C10 C14 1.380(13) . ? C11 C12 1.369(13) . ? C11 H10 0.9300 . ? C12 C13 1.386(15) . ? C12 H9 0.9300 . ? C13 C14 1.372(17) . ? C13 H8 0.9300 . ? C14 H7 0.9300 . ? C15 C16 1.392(13) . ? C15 H18 0.9300 . ? C16 C17 1.375(12) . ? C16 H17 0.9300 . ? C17 C18 1.369(10) . ? C17 H16 0.9300 . ? C18 H15 0.9300 . ? C19 C20 1.423(11) . ? C19 C23 1.425(11) . ? C19 C28 1.479(13) . ? C20 C21 1.414(12) . ? C20 C27 1.496(10) . ? C21 C22 1.420(10) . ? C21 C26 1.498(11) . ? C22 C23 1.419(12) . ? C22 C25 1.506(12) . ? C23 C24 1.498(10) . ? C24 H19 0.9600 . ? C24 H20 0.9600 . ? C24 H21 0.9600 . ? C25 H22 0.9600 . ? C25 H23 0.9600 . ? C25 H24 0.9600 . ? C26 H25 0.9600 . ? C26 H26 0.9600 . ? C26 H27 0.9600 . ? C27 H28 0.9600 . ? C27 H29 0.9600 . ? C27 H30 0.9600 . ? C28 H31 0.9600 . ? C28 H32 0.9600 . ? C28 H33 0.9600 . ? S1 O4 1.441(10) . ? S1 O6 1.476(10) . ? S1 O5 1.478(8) . ? S1 C29 1.718(13) . ? F1 C29 1.387(12) . ? F2 C29 1.286(12) . ? F3 C29 1.427(13) . ? N41 C41 1.205(16) . ? C41 C42 1.480(17) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? N51 C51 1.201(17) . ? C51 C52 1.486(17) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? N61 C61 1.264(17) . ? C61 C62 1.505(18) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? N71 C71 1.161(17) . ? C71 C72 1.539(17) . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 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 O2 Mo1 O3 105.5(3) . . ? O2 Mo1 O1 106.5(2) . . ? O3 Mo1 O1 106.3(3) . . ? O2 Mo1 C23 103.1(3) . . ? O3 Mo1 C23 90.8(3) . . ? O1 Mo1 C23 140.0(2) . . ? O2 Mo1 C19 84.7(3) . . ? O3 Mo1 C19 124.2(3) . . ? O1 Mo1 C19 123.4(3) . . ? C23 Mo1 C19 34.6(3) . . ? O2 Mo1 C22 136.9(3) . . ? O3 Mo1 C22 85.2(3) . . ? O1 Mo1 C22 110.1(3) . . ? C23 Mo1 C22 34.1(3) . . ? C19 Mo1 C22 56.4(3) . . ? O2 Mo1 C20 103.1(3) . . ? O3 Mo1 C20 140.6(2) . . ? O1 Mo1 C20 90.7(3) . . ? C23 Mo1 C20 56.4(2) . . ? C19 Mo1 C20 33.8(3) . . ? C22 Mo1 C20 55.4(3) . . ? O2 Mo1 C21 136.0(3) . . ? O3 Mo1 C21 112.4(3) . . ? O1 Mo1 C21 83.8(2) . . ? C23 Mo1 C21 56.2(3) . . ? C19 Mo1 C21 55.9(3) . . ? C22 Mo1 C21 33.3(2) . . ? C20 Mo1 C21 33.1(3) . . ? O1 Zn1 N3 103.9(3) . . ? O1 Zn1 N1 102.7(2) . . ? N3 Zn1 N1 117.9(3) . . ? O1 Zn1 N4 98.6(3) . . ? N3 Zn1 N4 114.9(3) . . ? N1 Zn1 N4 115.0(3) . . ? O1 Zn1 N2 175.7(3) . . ? N3 Zn1 N2 78.8(3) . . ? N1 Zn1 N2 78.6(3) . . ? N4 Zn1 N2 77.1(3) . . ? Mo1 O1 Zn1 145.2(3) . . ? C18 N1 C1 118.6(6) . . ? C18 N1 Zn1 125.3(5) . . ? C1 N1 Zn1 115.9(5) . . ? C3 N2 C9 113.9(7) . . ? C3 N2 C2 111.4(8) . . ? C9 N2 C2 112.4(7) . . ? C3 N2 Zn1 105.2(6) . . ? C9 N2 Zn1 107.5(6) . . ? C2 N2 Zn1 105.7(5) . . ? C4 N3 C5 119.2(9) . . ? C4 N3 Zn1 117.4(7) . . ? C5 N3 Zn1 123.3(7) . . ? C10 N4 C11 120.0(8) . . ? C10 N4 Zn1 117.3(6) . . ? C11 N4 Zn1 122.8(6) . . ? N1 C1 C15 121.3(8) . . ? N1 C1 C2 116.6(7) . . ? C15 C1 C2 122.1(8) . . ? N2 C2 C1 109.7(7) . . ? N2 C2 H13 109.7 . . ? C1 C2 H13 109.7 . . ? N2 C2 H14 109.7 . . ? C1 C2 H14 109.7 . . ? H13 C2 H14 108.2 . . ? N2 C3 C4 113.2(8) . . ? N2 C3 H5 108.9 . . ? C4 C3 H5 108.9 . . ? N2 C3 H6 108.9 . . ? C4 C3 H6 108.9 . . ? H5 C3 H6 107.8 . . ? N3 C4 C8 122.7(11) . . ? N3 C4 C3 116.6(9) . . ? C8 C4 C3 120.6(11) . . ? N3 C5 C6 120.9(11) . . ? N3 C5 H4 119.5 . . ? C6 C5 H4 119.5 . . ? C5 C6 C7 118.2(13) . . ? C5 C6 H3 120.9 . . ? C7 C6 H3 120.9 . . ? C8 C7 C6 120.9(12) . . ? C8 C7 H2 119.6 . . ? C6 C7 H2 119.6 . . ? C7 C8 C4 117.9(12) . . ? C7 C8 H1 121.0 . . ? C4 C8 H1 121.0 . . ? N2 C9 C10 110.1(8) . . ? N2 C9 H11 109.6 . . ? C10 C9 H11 109.6 . . ? N2 C9 H12 109.6 . . ? C10 C9 H12 109.6 . . ? H11 C9 H12 108.2 . . ? N4 C10 C14 120.1(9) . . ? N4 C10 C9 117.3(8) . . ? C14 C10 C9 122.5(9) . . ? N4 C11 C12 122.1(9) . . ? N4 C11 H10 119.0 . . ? C12 C11 H10 119.0 . . ? C11 C12 C13 118.1(10) . . ? C11 C12 H9 121.0 . . ? C13 C12 H9 121.0 . . ? C14 C13 C12 119.7(10) . . ? C14 C13 H8 120.2 . . ? C12 C13 H8 120.2 . . ? C13 C14 C10 120.1(10) . . ? C13 C14 H7 120.0 . . ? C10 C14 H7 120.0 . . ? C1 C15 C16 119.1(8) . . ? C1 C15 H18 120.4 . . ? C16 C15 H18 120.4 . . ? C17 C16 C15 118.7(7) . . ? C17 C16 H17 120.6 . . ? C15 C16 H17 120.6 . . ? C18 C17 C16 119.6(8) . . ? C18 C17 H16 120.2 . . ? C16 C17 H16 120.2 . . ? N1 C18 C17 122.6(7) . . ? N1 C18 H15 118.7 . . ? C17 C18 H15 118.7 . . ? C20 C19 C23 107.2(7) . . ? C20 C19 C28 125.9(8) . . ? C23 C19 C28 126.8(8) . . ? C20 C19 Mo1 75.1(5) . . ? C23 C19 Mo1 71.1(5) . . ? C28 C19 Mo1 121.6(5) . . ? C21 C20 C19 108.7(7) . . ? C21 C20 C27 126.0(7) . . ? C19 C20 C27 125.3(8) . . ? C21 C20 Mo1 74.4(4) . . ? C19 C20 Mo1 71.1(4) . . ? C27 C20 Mo1 123.2(5) . . ? C20 C21 C22 107.8(7) . . ? C20 C21 C26 126.0(7) . . ? C22 C21 C26 126.2(8) . . ? C20 C21 Mo1 72.5(4) . . ? C22 C21 Mo1 71.7(4) . . ? C26 C21 Mo1 121.2(6) . . ? C23 C22 C21 108.0(7) . . ? C23 C22 C25 125.5(7) . . ? C21 C22 C25 126.5(8) . . ? C23 C22 Mo1 70.0(4) . . ? C21 C22 Mo1 75.0(4) . . ? C25 C22 Mo1 119.6(6) . . ? C22 C23 C19 108.2(7) . . ? C22 C23 C24 125.0(8) . . ? C19 C23 C24 126.7(8) . . ? C22 C23 Mo1 75.9(5) . . ? C19 C23 Mo1 74.3(4) . . ? C24 C23 Mo1 117.3(5) . . ? C23 C24 H19 109.5 . . ? C23 C24 H20 109.5 . . ? H19 C24 H20 109.5 . . ? C23 C24 H21 109.5 . . ? H19 C24 H21 109.5 . . ? H20 C24 H21 109.5 . . ? C22 C25 H22 109.5 . . ? C22 C25 H23 109.5 . . ? H22 C25 H23 109.5 . . ? C22 C25 H24 109.5 . . ? H22 C25 H24 109.5 . . ? H23 C25 H24 109.5 . . ? C21 C26 H25 109.5 . . ? C21 C26 H26 109.5 . . ? H25 C26 H26 109.5 . . ? C21 C26 H27 109.5 . . ? H25 C26 H27 109.5 . . ? H26 C26 H27 109.5 . . ? C20 C27 H28 109.5 . . ? C20 C27 H29 109.5 . . ? H28 C27 H29 109.5 . . ? C20 C27 H30 109.5 . . ? H28 C27 H30 109.5 . . ? H29 C27 H30 109.5 . . ? C19 C28 H31 109.5 . . ? C19 C28 H32 109.5 . . ? H31 C28 H32 109.5 . . ? C19 C28 H33 109.5 . . ? H31 C28 H33 109.5 . . ? H32 C28 H33 109.5 . . ? O4 S1 O6 114.0(6) . . ? O4 S1 O5 116.7(6) . . ? O6 S1 O5 117.2(6) . . ? O4 S1 C29 104.9(7) . . ? O6 S1 C29 100.8(6) . . ? O5 S1 C29 99.7(5) . . ? F2 C29 F1 109.5(9) . . ? F2 C29 F3 102.0(10) . . ? F1 C29 F3 98.6(9) . . ? F2 C29 S1 120.4(9) . . ? F1 C29 S1 110.8(8) . . ? F3 C29 S1 113.1(8) . . ? N41 C41 C42 168(5) . . ? N51 C51 C52 165(5) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N61 C61 C62 154(4) . . ? N71 C71 C72 160(4) . . ? _diffrn_measured_fraction_theta_max .998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full .998 _refine_diff_density_max 1.916 _refine_diff_density_min -1.232 _refine_diff_density_rms .140 _database_code_depnum_ccdc_archive 'CCDC 936996' ####################################################################### # # 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_jf137 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C28 H33 Co Mo N4 O3), 2(C F3 O3 S), 1/2(C4 H10 O), C2 H3 N' _chemical_formula_sum 'C62 H74 Co2 F6 Mo2 N9 O12.50 S2' _chemical_formula_weight 1633.16 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 'P 21/c' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' 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 14.1365(4) _cell_length_b 14.2503(6) _cell_length_c 37.6652(10) _cell_angle_alpha 90.00 _cell_angle_beta 108.3110(19) _cell_angle_gamma 90.00 _cell_volume 7203.4(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 43769 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 26.67 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3332 _exptl_absorpt_coefficient_mu 0.929 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7308 _exptl_absorpt_correction_T_max 0.9638 _exptl_absorpt_process_details 'X-AREA (Stoe & Cie, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'long fine focus sealed X-ray tube' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_collimation '0.5 mm diameter monocapillary' _diffrn_measurement_device 'Stoe IPDS-2t diffractometer' _diffrn_measurement_method '\w-rotation,\w-incr.=1\%,319 exposures' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 54821 _diffrn_reflns_av_R_equivalents 0.1034 _diffrn_reflns_av_sigmaI/netI 0.0757 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12263 _reflns_number_gt 9057 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-RED (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON, 1990' _computing_publication_material 'PLATON, 1990' _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^)+(0.0700P)^2^+92.0000P] 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 12263 _refine_ls_number_parameters 870 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1030 _refine_ls_R_factor_gt 0.0805 _refine_ls_wR_factor_ref 0.2151 _refine_ls_wR_factor_gt 0.2049 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.016 _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 0.43027(5) 0.66101(5) 0.21981(2) 0.01974(19) Uani 1 1 d . . . Co1 Co 0.39520(8) 0.50588(8) 0.14193(3) 0.0214(3) Uani 1 1 d . . . O1 O 0.4523(4) 0.5846(4) 0.18485(18) 0.0260(13) Uani 1 1 d . . . O2 O 0.3948(5) 0.5892(4) 0.25027(18) 0.0289(14) Uani 1 1 d . . . O3 O 0.3253(4) 0.7252(4) 0.19648(18) 0.0255(13) Uani 1 1 d . . . N1 N 0.3294(6) 0.6009(5) 0.1006(2) 0.0299(17) Uani 1 1 d . . . N2 N 0.3362(6) 0.4161(5) 0.0923(2) 0.0281(17) Uani 1 1 d . . . N3 N 0.5208(5) 0.4403(5) 0.1382(2) 0.0205(15) Uani 1 1 d . . . C5 C 0.3076(7) 0.5711(7) 0.0651(3) 0.033(2) Uani 1 1 d . . . C6 C 0.3370(8) 0.4732(7) 0.0594(3) 0.033(2) Uani 1 1 d . . . H6A H 0.2897 0.4466 0.0363 0.040 Uiso 1 1 calc R . . H6B H 0.4045 0.4727 0.0567 0.040 Uiso 1 1 calc R . . C13 C 0.4043(7) 0.3332(6) 0.0971(3) 0.029(2) Uani 1 1 d . . . H13A H 0.4016 0.3083 0.0723 0.035 Uiso 1 1 calc R . . H13B H 0.3820 0.2830 0.1109 0.035 Uiso 1 1 calc R . . C14 C 0.5095(7) 0.3605(6) 0.1184(3) 0.0263(19) Uani 1 1 d . . . C18 C 0.6130(6) 0.4667(6) 0.1571(2) 0.0244(18) Uani 1 1 d . . . H18 H 0.6216 0.5246 0.1702 0.029 Uiso 1 1 calc R . . C17 C 0.6968(7) 0.4157(6) 0.1589(3) 0.029(2) Uani 1 1 d . . . H17 H 0.7610 0.4375 0.1732 0.034 Uiso 1 1 calc R . . C16 C 0.6854(7) 0.3313(6) 0.1394(3) 0.034(2) Uani 1 1 d . . . H16 H 0.7415 0.2937 0.1400 0.041 Uiso 1 1 calc R . . C15 C 0.5897(7) 0.3039(6) 0.1189(3) 0.032(2) Uani 1 1 d . . . H15 H 0.5791 0.2467 0.1053 0.039 Uiso 1 1 calc R . . C7 C 0.2362(7) 0.3878(7) 0.0907(3) 0.033(2) Uani 1 1 d . . . H7A H 0.2168 0.3307 0.0751 0.039 Uiso 1 1 calc R . . H7B H 0.1884 0.4383 0.0791 0.039 Uiso 1 1 calc R . . C8 C 0.2332(7) 0.3681(6) 0.1299(3) 0.028(2) Uani 1 1 d . . . N4 N 0.2982(5) 0.4183(5) 0.1573(2) 0.0252(16) Uani 1 1 d . . . C12 C 0.2985(6) 0.4068(6) 0.1927(3) 0.0227(18) Uani 1 1 d . . . H12 H 0.3434 0.4432 0.2118 0.027 Uiso 1 1 calc R . . C11 C 0.2363(7) 0.3441(6) 0.2025(3) 0.030(2) Uani 1 1 d . . . H11 H 0.2398 0.3357 0.2279 0.036 Uiso 1 1 calc R . . C10 C 0.1674(7) 0.2930(6) 0.1736(3) 0.031(2) Uani 1 1 d . . . H10 H 0.1219 0.2509 0.1791 0.037 Uiso 1 1 calc R . . C9 C 0.1671(7) 0.3051(6) 0.1375(3) 0.033(2) Uani 1 1 d . . . H9 H 0.1220 0.2705 0.1178 0.040 Uiso 1 1 calc R . . C4 C 0.2608(9) 0.6284(8) 0.0350(3) 0.045(3) Uani 1 1 d . . . H4 H 0.2435 0.6059 0.0100 0.053 Uiso 1 1 calc R . . C3 C 0.2396(10) 0.7221(8) 0.0429(3) 0.055(3) Uani 1 1 d . . . H3 H 0.2100 0.7644 0.0230 0.066 Uiso 1 1 calc R . . C2 C 0.2618(9) 0.7507(8) 0.0787(3) 0.047(3) Uani 1 1 d . . . H2 H 0.2468 0.8129 0.0842 0.057 Uiso 1 1 calc R . . C1 C 0.3067(9) 0.6888(7) 0.1075(3) 0.041(2) Uani 1 1 d . . . H1 H 0.3217 0.7092 0.1326 0.049 Uiso 1 1 calc R . . C19 C 0.5601(6) 0.7133(5) 0.2751(2) 0.0203(17) Uani 1 1 d . . . C23 C 0.5013(6) 0.7933(6) 0.2575(3) 0.0256(19) Uani 1 1 d . . . C22 C 0.5192(6) 0.8104(6) 0.2229(3) 0.0230(18) Uani 1 1 d . . . C21 C 0.5851(6) 0.7402(6) 0.2179(3) 0.0221(18) Uani 1 1 d . . . C20 C 0.6093(6) 0.6812(6) 0.2501(3) 0.0232(18) Uani 1 1 d . . . C25 C 0.6814(7) 0.5996(6) 0.2576(3) 0.0266(19) Uani 1 1 d . . . H25A H 0.7492 0.6225 0.2698 0.040 Uiso 1 1 calc R . . H25B H 0.6781 0.5692 0.2339 0.040 Uiso 1 1 calc R . . H25C H 0.6635 0.5542 0.2740 0.040 Uiso 1 1 calc R . . C26 C 0.6211(7) 0.7306(6) 0.1844(3) 0.0263(19) Uani 1 1 d . . . H26A H 0.5710 0.6971 0.1645 0.039 Uiso 1 1 calc R . . H26B H 0.6838 0.6953 0.1915 0.039 Uiso 1 1 calc R . . H26C H 0.6319 0.7931 0.1755 0.039 Uiso 1 1 calc R . . C27 C 0.4737(7) 0.8894(6) 0.1971(3) 0.029(2) Uani 1 1 d . . . H27A H 0.5072 0.9482 0.2073 0.044 Uiso 1 1 calc R . . H27B H 0.4027 0.8942 0.1946 0.044 Uiso 1 1 calc R . . H27C H 0.4813 0.8777 0.1725 0.044 Uiso 1 1 calc R . . C28 C 0.4344(7) 0.8516(6) 0.2731(3) 0.032(2) Uani 1 1 d . . . H28A H 0.4215 0.8177 0.2938 0.048 Uiso 1 1 calc R . . H28B H 0.3712 0.8635 0.2534 0.048 Uiso 1 1 calc R . . H28C H 0.4670 0.9115 0.2823 0.048 Uiso 1 1 calc R . . C24 C 0.5694(7) 0.6751(6) 0.3125(3) 0.031(2) Uani 1 1 d . . . H24A H 0.5556 0.6075 0.3105 0.046 Uiso 1 1 calc R . . H24B H 0.5215 0.7064 0.3225 0.046 Uiso 1 1 calc R . . H24C H 0.6371 0.6858 0.3293 0.046 Uiso 1 1 calc R . . Mo2 Mo 0.07255(5) 0.15914(5) 0.27867(2) 0.01880(19) Uani 1 1 d . . . Co2 Co 0.12322(8) 0.31024(7) 0.35920(3) 0.0199(3) Uani 1 1 d . . . O4 O 0.0602(4) 0.2319(4) 0.31646(18) 0.0247(13) Uani 1 1 d . . . O5 O 0.1102(4) 0.2332(4) 0.24912(17) 0.0249(13) Uani 1 1 d . . . O6 O 0.1735(4) 0.0872(4) 0.29918(18) 0.0258(13) Uani 1 1 d . . . N6 N 0.1876(5) 0.3990(5) 0.4094(2) 0.0244(16) Uani 1 1 d . . . C35 C 0.2838(6) 0.4355(6) 0.4077(2) 0.0251(19) Uani 1 1 d . . . H35A H 0.3369 0.3888 0.4185 0.030 Uiso 1 1 calc R . . H35B H 0.3009 0.4938 0.4226 0.030 Uiso 1 1 calc R . . C36 C 0.2776(6) 0.4554(6) 0.3678(3) 0.0227(18) Uani 1 1 d . . . N7 N 0.2118(5) 0.4032(5) 0.3415(2) 0.0202(15) Uani 1 1 d . . . C40 C 0.2059(6) 0.4153(5) 0.3059(2) 0.0216(18) Uani 1 1 d . . . H40 H 0.1595 0.3785 0.2874 0.026 Uiso 1 1 calc R . . C39 C 0.2644(6) 0.4789(6) 0.2945(2) 0.0222(18) Uani 1 1 d . . . H39 H 0.2592 0.4849 0.2688 0.027 Uiso 1 1 calc R . . C38 C 0.3308(6) 0.5337(6) 0.3213(3) 0.0264(19) Uani 1 1 d . . . H38 H 0.3712 0.5786 0.3142 0.032 Uiso 1 1 calc R . . C37 C 0.3374(6) 0.5221(6) 0.3587(3) 0.0262(19) Uani 1 1 d . . . H37 H 0.3821 0.5591 0.3776 0.031 Uiso 1 1 calc R . . C34 C 0.1986(7) 0.3367(6) 0.4413(3) 0.0276(19) Uani 1 1 d . . . H34A H 0.1333 0.3288 0.4454 0.033 Uiso 1 1 calc R . . H34B H 0.2452 0.3652 0.4641 0.033 Uiso 1 1 calc R . . C33 C 0.2370(7) 0.2439(6) 0.4346(3) 0.0246(19) Uani 1 1 d . . . N5 N 0.2072(6) 0.2168(5) 0.3982(2) 0.0270(17) Uani 1 1 d . . . C29 C 0.2385(7) 0.1310(6) 0.3894(3) 0.029(2) Uani 1 1 d . . . H29 H 0.2181 0.1107 0.3641 0.035 Uiso 1 1 calc R . . C30 C 0.2984(7) 0.0747(6) 0.4165(3) 0.032(2) Uani 1 1 d . . . H30 H 0.3183 0.0152 0.4099 0.038 Uiso 1 1 calc R . . C31 C 0.3308(8) 0.1035(7) 0.4536(3) 0.036(2) Uani 1 1 d . . . H31 H 0.3733 0.0644 0.4723 0.043 Uiso 1 1 calc R . . C32 C 0.3008(7) 0.1889(6) 0.4629(3) 0.032(2) Uani 1 1 d . . . H32 H 0.3229 0.2104 0.4880 0.038 Uiso 1 1 calc R . . C41 C 0.1175(6) 0.4768(6) 0.4073(3) 0.0238(18) Uani 1 1 d . . . H41A H 0.1323 0.5287 0.3924 0.029 Uiso 1 1 calc R . . H41B H 0.1262 0.5007 0.4329 0.029 Uiso 1 1 calc R . . C42 C 0.0112(7) 0.4450(6) 0.3897(2) 0.0237(18) Uani 1 1 d . . . N8 N -0.0020(5) 0.3685(5) 0.3679(2) 0.0224(15) Uani 1 1 d . . . C46 C -0.0956(7) 0.3389(6) 0.3497(3) 0.029(2) Uani 1 1 d . . . H46 H -0.1050 0.2858 0.3337 0.035 Uiso 1 1 calc R . . C45 C -0.1783(7) 0.3840(7) 0.3539(3) 0.034(2) Uani 1 1 d . . . H45 H -0.2433 0.3608 0.3415 0.041 Uiso 1 1 calc R . . C44 C -0.1654(7) 0.4622(6) 0.3760(3) 0.034(2) Uani 1 1 d . . . H44 H -0.2214 0.4953 0.3784 0.041 Uiso 1 1 calc R . . C43 C -0.0690(7) 0.4927(6) 0.3949(3) 0.032(2) Uani 1 1 d . . . H43 H -0.0583 0.5453 0.4112 0.039 Uiso 1 1 calc R . . C47 C -0.1095(6) 0.1482(5) 0.2498(2) 0.0207(18) Uani 1 1 d . . . C48 C -0.0644(6) 0.1193(6) 0.2230(2) 0.0260(19) Uani 1 1 d . . . C49 C -0.0080(6) 0.0352(6) 0.2375(2) 0.0218(18) Uani 1 1 d . . . C50 C -0.0231(6) 0.0130(5) 0.2724(3) 0.0220(18) Uani 1 1 d . . . C51 C -0.0839(6) 0.0831(5) 0.2802(2) 0.0204(17) Uani 1 1 d . . . C52 C -0.1158(6) 0.0876(6) 0.3143(3) 0.0268(19) Uani 1 1 d . . . H52A H -0.0999 0.0282 0.3280 0.040 Uiso 1 1 calc R . . H52B H -0.1878 0.0987 0.3070 0.040 Uiso 1 1 calc R . . H52C H -0.0807 0.1390 0.3304 0.040 Uiso 1 1 calc R . . C56 C 0.0184(7) -0.0709(6) 0.2954(3) 0.029(2) Uani 1 1 d . . . H56A H 0.0180 -0.0606 0.3211 0.044 Uiso 1 1 calc R . . H56B H 0.0869 -0.0815 0.2954 0.044 Uiso 1 1 calc R . . H56C H -0.0224 -0.1259 0.2849 0.044 Uiso 1 1 calc R . . C55 C 0.0519(7) -0.0207(6) 0.2185(3) 0.030(2) Uani 1 1 d . . . H55A H 0.1194 -0.0297 0.2358 0.044 Uiso 1 1 calc R . . H55B H 0.0551 0.0129 0.1963 0.044 Uiso 1 1 calc R . . H55C H 0.0203 -0.0820 0.2112 0.044 Uiso 1 1 calc R . . C54 C -0.0757(7) 0.1639(6) 0.1862(3) 0.029(2) Uani 1 1 d . . . H54A H -0.1382 0.1430 0.1679 0.044 Uiso 1 1 calc R . . H54B H -0.0196 0.1457 0.1776 0.044 Uiso 1 1 calc R . . H54C H -0.0766 0.2323 0.1888 0.044 Uiso 1 1 calc R . . C53 C -0.1774(6) 0.2319(6) 0.2461(3) 0.0266(19) Uani 1 1 d . . . H53A H -0.1380 0.2868 0.2576 0.040 Uiso 1 1 calc R . . H53B H -0.2269 0.2186 0.2587 0.040 Uiso 1 1 calc R . . H53C H -0.2114 0.2445 0.2195 0.040 Uiso 1 1 calc R . . O13 O 0.9916(9) 0.7436(8) 0.0345(4) 0.030(3) Uiso 0.50 1 d PD . . C59 C 0.9804(16) 0.8825(12) -0.0012(6) 0.040(3) Uiso 0.50 1 d PD . . H59A H 0.9471 0.9150 0.0145 0.060 Uiso 0.50 1 calc PR . . H59B H 0.9569 0.9083 -0.0266 0.060 Uiso 0.50 1 calc PR . . H59C H 1.0526 0.8916 0.0093 0.060 Uiso 0.50 1 calc PR . . C60 C 0.957(2) 0.7809(14) -0.0023(6) 0.057(4) Uiso 0.50 1 d PD . . H60A H 0.8843 0.7713 -0.0129 0.068 Uiso 0.50 1 calc PR . . H60B H 0.9898 0.7479 -0.0184 0.068 Uiso 0.50 1 calc PR . . C61 C 0.982(2) 0.6441(15) 0.0386(6) 0.057(4) Uiso 0.50 1 d PD . . H61A H 1.0214 0.6108 0.0249 0.068 Uiso 0.50 1 calc PR . . H61B H 0.9115 0.6257 0.0275 0.068 Uiso 0.50 1 calc PR . . C62 C 1.0185(16) 0.6157(15) 0.0791(5) 0.040(3) Uiso 0.50 1 d PD . . H62A H 1.0790 0.6511 0.0921 0.060 Uiso 0.50 1 calc PR . . H62B H 1.0333 0.5484 0.0810 0.060 Uiso 0.50 1 calc PR . . H62C H 0.9668 0.6293 0.0907 0.060 Uiso 0.50 1 calc PR . . S1 S 0.86522(17) 0.21877(16) 0.07845(7) 0.0289(5) Uani 1 1 d . . . F1 F 0.9423(6) 0.3751(4) 0.0643(2) 0.0580(19) Uani 1 1 d . . . F2 F 0.8969(5) 0.3794(4) 0.11398(18) 0.0530(17) Uani 1 1 d . . . F3 F 0.7856(5) 0.3843(4) 0.05957(19) 0.0516(17) Uani 1 1 d . . . O7 O 0.8388(6) 0.1974(5) 0.0392(2) 0.0418(17) Uani 1 1 d . . . O8 O 0.7873(5) 0.1982(5) 0.0943(2) 0.0379(16) Uani 1 1 d . . . O9 O 0.9630(5) 0.1911(4) 0.1006(2) 0.0369(16) Uani 1 1 d . . . C57 C 0.8727(8) 0.3451(7) 0.0796(3) 0.039(2) Uani 1 1 d . . . S2 S 0.3649(2) 0.10117(18) 0.06283(8) 0.0394(6) Uani 1 1 d . . . F4 F 0.2552(10) -0.0370(7) 0.0278(5) 0.155(7) Uani 1 1 d . . . F5 F 0.3758(14) -0.0092(9) 0.0089(4) 0.158(6) Uani 1 1 d . . . F6 F 0.4010(9) -0.0785(6) 0.0616(4) 0.122(4) Uani 1 1 d . . . O10 O 0.3158(8) 0.1631(6) 0.0332(2) 0.067(3) Uani 1 1 d . . . O11 O 0.4686(7) 0.1147(6) 0.0759(4) 0.106(5) Uani 1 1 d . . . O12 O 0.3186(14) 0.0895(10) 0.0904(4) 0.132(6) Uani 1 1 d . . . C58 C 0.3526(17) -0.0113(10) 0.0402(5) 0.089(6) Uani 1 1 d . . . N9 N 0.5404(7) 0.3910(7) 0.0302(3) 0.051(3) Uani 1 1 d . . . C64 C 0.5550(8) 0.3186(9) 0.0241(3) 0.044(3) Uani 1 1 d . . . C63 C 0.5765(9) 0.2218(8) 0.0145(4) 0.055(3) Uani 1 1 d . . . H63A H 0.5280 0.1785 0.0192 0.083 Uiso 1 1 calc R . . H63B H 0.6438 0.2039 0.0300 0.083 Uiso 1 1 calc R . . H63C H 0.5721 0.2190 -0.0120 0.083 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 0.0189(4) 0.0169(4) 0.0241(4) -0.0019(3) 0.0078(3) -0.0021(3) Co1 0.0216(6) 0.0196(6) 0.0226(6) -0.0002(5) 0.0063(5) -0.0002(4) O1 0.024(3) 0.025(3) 0.030(4) -0.003(3) 0.010(3) 0.000(2) O2 0.030(3) 0.026(3) 0.030(4) -0.003(3) 0.009(3) -0.009(3) O3 0.023(3) 0.018(3) 0.033(4) -0.001(3) 0.006(3) -0.001(2) N1 0.032(4) 0.030(4) 0.029(5) 0.003(3) 0.012(3) 0.008(3) N2 0.027(4) 0.026(4) 0.030(5) -0.002(3) 0.007(3) -0.001(3) N3 0.023(4) 0.019(3) 0.019(4) 0.003(3) 0.007(3) -0.000(3) C5 0.030(5) 0.038(5) 0.031(6) 0.004(4) 0.011(4) 0.006(4) C6 0.043(6) 0.037(5) 0.020(5) 0.005(4) 0.010(4) 0.003(4) C13 0.035(5) 0.023(4) 0.024(5) -0.005(4) 0.002(4) 0.001(4) C14 0.028(5) 0.026(4) 0.026(5) -0.001(4) 0.009(4) -0.002(4) C18 0.030(5) 0.023(4) 0.017(4) -0.002(3) 0.004(4) -0.002(4) C17 0.021(4) 0.029(5) 0.035(6) 0.006(4) 0.009(4) -0.002(4) C16 0.036(5) 0.026(5) 0.042(6) 0.003(4) 0.017(5) 0.012(4) C15 0.044(6) 0.019(4) 0.040(6) -0.001(4) 0.021(5) 0.002(4) C7 0.030(5) 0.033(5) 0.029(5) -0.001(4) -0.001(4) -0.008(4) C8 0.023(4) 0.027(5) 0.035(6) -0.006(4) 0.008(4) -0.003(4) N4 0.019(4) 0.024(4) 0.029(4) 0.002(3) 0.004(3) 0.001(3) C12 0.020(4) 0.023(4) 0.025(5) -0.002(3) 0.007(3) 0.000(3) C11 0.026(5) 0.021(4) 0.045(6) 0.003(4) 0.016(4) 0.003(4) C10 0.028(5) 0.023(5) 0.045(6) -0.000(4) 0.014(4) -0.002(4) C9 0.024(5) 0.026(5) 0.044(6) -0.005(4) 0.003(4) -0.009(4) C4 0.056(7) 0.049(6) 0.030(6) 0.009(5) 0.015(5) 0.011(5) C3 0.079(9) 0.045(7) 0.041(7) 0.019(5) 0.020(6) 0.030(6) C2 0.066(8) 0.044(6) 0.033(7) 0.009(5) 0.018(6) 0.017(5) C1 0.057(7) 0.038(6) 0.030(6) 0.002(4) 0.016(5) 0.012(5) C19 0.019(4) 0.017(4) 0.022(5) -0.003(3) 0.003(3) -0.007(3) C23 0.024(4) 0.018(4) 0.037(6) -0.009(4) 0.012(4) -0.001(3) C22 0.022(4) 0.017(4) 0.029(5) -0.003(3) 0.007(4) -0.005(3) C21 0.016(4) 0.024(4) 0.028(5) -0.000(3) 0.008(3) -0.006(3) C20 0.020(4) 0.020(4) 0.028(5) -0.003(3) 0.006(4) -0.006(3) C25 0.026(4) 0.023(4) 0.031(5) -0.003(4) 0.009(4) -0.001(4) C26 0.025(4) 0.024(4) 0.031(5) 0.001(4) 0.010(4) -0.008(3) C27 0.032(5) 0.018(4) 0.039(6) 0.000(4) 0.012(4) -0.002(4) C28 0.030(5) 0.023(5) 0.047(6) -0.013(4) 0.015(4) -0.004(4) C24 0.035(5) 0.026(5) 0.028(5) -0.007(4) 0.007(4) -0.007(4) Mo2 0.0180(4) 0.0166(4) 0.0212(4) -0.0015(3) 0.0054(3) -0.0017(3) Co2 0.0217(6) 0.0169(5) 0.0207(6) -0.0009(4) 0.0063(5) -0.0008(4) O4 0.023(3) 0.022(3) 0.030(4) -0.004(2) 0.010(3) -0.000(2) O5 0.025(3) 0.023(3) 0.028(4) -0.001(2) 0.009(3) -0.003(2) O6 0.019(3) 0.025(3) 0.034(4) -0.003(3) 0.009(3) -0.002(2) N6 0.020(4) 0.023(4) 0.031(4) -0.004(3) 0.008(3) -0.004(3) C35 0.022(4) 0.030(5) 0.020(5) -0.001(4) 0.002(4) -0.004(3) C36 0.019(4) 0.021(4) 0.027(5) 0.001(3) 0.005(4) 0.006(3) N7 0.021(4) 0.019(3) 0.020(4) 0.000(3) 0.005(3) 0.001(3) C40 0.023(4) 0.015(4) 0.025(5) 0.001(3) 0.004(4) 0.008(3) C39 0.019(4) 0.025(4) 0.021(5) 0.003(3) 0.005(3) 0.003(3) C38 0.021(4) 0.021(4) 0.038(6) 0.002(4) 0.010(4) 0.002(3) C37 0.021(4) 0.022(4) 0.035(5) -0.003(4) 0.008(4) -0.005(3) C34 0.033(5) 0.024(4) 0.027(5) -0.000(4) 0.011(4) 0.000(4) C33 0.032(5) 0.018(4) 0.022(5) 0.000(3) 0.006(4) -0.000(3) N5 0.033(4) 0.021(4) 0.028(4) 0.002(3) 0.010(3) 0.001(3) C29 0.044(6) 0.023(4) 0.019(5) -0.003(3) 0.008(4) -0.003(4) C30 0.035(5) 0.024(5) 0.034(6) 0.002(4) 0.008(4) 0.004(4) C31 0.043(6) 0.030(5) 0.035(6) 0.010(4) 0.014(5) 0.005(4) C32 0.039(5) 0.026(5) 0.025(5) -0.001(4) 0.004(4) 0.003(4) C41 0.023(4) 0.018(4) 0.028(5) -0.005(3) 0.005(4) -0.004(3) C42 0.028(5) 0.023(4) 0.020(5) 0.002(3) 0.008(4) -0.005(3) N8 0.024(4) 0.016(3) 0.027(4) -0.001(3) 0.008(3) -0.000(3) C46 0.031(5) 0.019(4) 0.042(6) 0.002(4) 0.016(4) 0.002(4) C45 0.024(5) 0.036(5) 0.041(6) 0.003(4) 0.009(4) -0.005(4) C44 0.030(5) 0.026(5) 0.049(6) -0.000(4) 0.018(5) 0.001(4) C43 0.038(5) 0.024(5) 0.036(6) -0.007(4) 0.012(4) -0.002(4) C47 0.013(4) 0.016(4) 0.030(5) -0.003(3) 0.003(3) -0.001(3) C48 0.024(4) 0.034(5) 0.016(5) 0.002(4) -0.001(3) -0.006(4) C49 0.014(4) 0.018(4) 0.030(5) -0.009(3) 0.002(3) -0.011(3) C50 0.018(4) 0.015(4) 0.030(5) -0.002(3) 0.002(3) -0.003(3) C51 0.018(4) 0.017(4) 0.025(5) -0.004(3) 0.006(3) -0.005(3) C52 0.023(4) 0.025(4) 0.033(5) 0.001(4) 0.009(4) 0.000(3) C56 0.026(5) 0.020(4) 0.038(6) 0.003(4) 0.005(4) -0.001(3) C55 0.027(5) 0.029(5) 0.032(5) -0.007(4) 0.008(4) -0.000(4) C54 0.032(5) 0.027(5) 0.025(5) 0.003(4) 0.003(4) -0.005(4) C53 0.024(4) 0.022(4) 0.034(5) 0.002(4) 0.009(4) 0.004(3) S1 0.0315(12) 0.0265(11) 0.0279(13) -0.0017(9) 0.0082(10) 0.0018(9) F1 0.076(5) 0.036(3) 0.072(5) 0.006(3) 0.039(4) -0.007(3) F2 0.077(5) 0.039(3) 0.038(4) -0.010(3) 0.012(3) 0.001(3) F3 0.066(4) 0.037(3) 0.046(4) 0.002(3) 0.010(3) 0.023(3) O7 0.059(5) 0.038(4) 0.027(4) -0.005(3) 0.012(3) -0.001(3) O8 0.039(4) 0.033(4) 0.045(4) -0.001(3) 0.017(3) 0.001(3) O9 0.025(3) 0.029(3) 0.053(5) -0.001(3) 0.006(3) -0.002(3) C57 0.051(6) 0.032(5) 0.034(6) -0.002(4) 0.012(5) 0.004(5) S2 0.0443(15) 0.0360(13) 0.0335(15) 0.0031(11) 0.0059(11) -0.0061(11) F4 0.133(10) 0.054(6) 0.212(15) -0.014(7) -0.038(10) -0.047(6) F5 0.269(19) 0.095(9) 0.129(12) -0.026(8) 0.089(12) 0.057(10) F6 0.146(10) 0.041(5) 0.147(11) 0.005(6) 0.001(8) 0.011(5) O10 0.099(7) 0.037(4) 0.042(5) 0.003(4) -0.009(5) -0.004(4) O11 0.053(6) 0.041(5) 0.174(13) 0.018(6) -0.038(7) -0.003(4) O12 0.212(17) 0.112(10) 0.129(12) -0.022(9) 0.134(13) -0.061(11) C58 0.143(17) 0.037(8) 0.078(12) -0.001(7) 0.024(11) 0.001(9) N9 0.051(6) 0.040(6) 0.049(6) -0.002(4) -0.002(5) -0.006(4) C64 0.043(6) 0.049(7) 0.035(6) 0.000(5) 0.006(5) 0.003(5) C63 0.053(7) 0.041(6) 0.066(9) -0.009(6) 0.009(6) -0.000(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 O2 1.725(6) . ? Mo1 O3 1.730(6) . ? Mo1 O1 1.809(6) . ? Mo1 C23 2.384(8) . ? Mo1 C19 2.422(8) . ? Mo1 C20 2.444(8) . ? Mo1 C22 2.456(8) . ? Mo1 C21 2.484(8) . ? Co1 O1 1.925(6) . ? Co1 N3 2.049(7) . ? Co1 N1 2.053(8) . ? Co1 N4 2.067(7) . ? Co1 N2 2.201(8) . ? N1 C1 1.338(13) . ? N1 C5 1.342(13) . ? N2 C7 1.453(12) . ? N2 C6 1.485(12) . ? N2 C13 1.500(11) . ? N3 C18 1.328(11) . ? N3 C14 1.343(11) . ? C5 C4 1.386(14) . ? C5 C6 1.490(13) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C13 C14 1.502(12) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.386(13) . ? C18 C17 1.373(13) . ? C18 H18 0.9500 . ? C17 C16 1.393(14) . ? C17 H17 0.9500 . ? C16 C15 1.387(14) . ? C16 H16 0.9500 . ? C15 H15 0.9500 . ? C7 C8 1.517(14) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N4 1.351(12) . ? C8 C9 1.389(13) . ? N4 C12 1.341(12) . ? C12 C11 1.383(12) . ? C12 H12 0.9500 . ? C11 C10 1.414(14) . ? C11 H11 0.9500 . ? C10 C9 1.369(15) . ? C10 H10 0.9500 . ? C9 H9 0.9500 . ? C4 C3 1.419(16) . ? C4 H4 0.9500 . ? C3 C2 1.349(17) . ? C3 H3 0.9500 . ? C2 C1 1.387(15) . ? C2 H2 0.9500 . ? C1 H1 0.9500 . ? C19 C20 1.410(12) . ? C19 C23 1.444(12) . ? C19 C24 1.477(13) . ? C23 C22 1.423(13) . ? C23 C28 1.511(12) . ? C22 C21 1.421(12) . ? C22 C27 1.494(12) . ? C21 C20 1.429(12) . ? C21 C26 1.505(13) . ? C20 C25 1.513(12) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? Mo2 O6 1.730(6) . ? Mo2 O5 1.734(6) . ? Mo2 O4 1.813(6) . ? Mo2 C49 2.390(8) . ? Mo2 C48 2.433(8) . ? Mo2 C50 2.453(8) . ? Mo2 C47 2.464(8) . ? Mo2 C51 2.479(8) . ? Co2 O4 1.931(6) . ? Co2 N5 2.060(7) . ? Co2 N8 2.072(7) . ? Co2 N7 2.072(7) . ? Co2 N6 2.218(7) . ? N6 C34 1.464(12) . ? N6 C41 1.473(11) . ? N6 C35 1.475(11) . ? C35 C36 1.505(13) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 N7 1.350(11) . ? C36 C37 1.385(12) . ? N7 C40 1.328(11) . ? C40 C39 1.382(12) . ? C40 H40 0.9500 . ? C39 C38 1.383(12) . ? C39 H39 0.9500 . ? C38 C37 1.392(14) . ? C38 H38 0.9500 . ? C37 H37 0.9500 . ? C34 C33 1.481(12) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C33 N5 1.357(12) . ? C33 C32 1.399(13) . ? N5 C29 1.377(12) . ? C29 C30 1.363(13) . ? C29 H29 0.9500 . ? C30 C31 1.389(14) . ? C30 H30 0.9500 . ? C31 C32 1.371(14) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C41 C42 1.509(12) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 N8 1.344(11) . ? C42 C43 1.387(13) . ? N8 C46 1.352(12) . ? C46 C45 1.385(13) . ? C46 H46 0.9500 . ? C45 C44 1.369(14) . ? C45 H45 0.9500 . ? C44 C43 1.395(14) . ? C44 H44 0.9500 . ? C43 H43 0.9500 . ? C47 C48 1.414(13) . ? C47 C51 1.430(12) . ? C47 C53 1.509(11) . ? C48 C49 1.448(12) . ? C48 C54 1.487(13) . ? C49 C50 1.431(13) . ? C49 C55 1.496(12) . ? C50 C51 1.407(12) . ? C50 C56 1.486(12) . ? C51 C52 1.491(13) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? O13 C60 1.42(2) . ? O13 C61 1.44(2) . ? C59 C60 1.484(17) . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.506(18) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? S1 O9 1.427(7) . ? S1 O7 1.438(7) . ? S1 O8 1.439(7) . ? S1 C57 1.804(10) . ? F1 C57 1.356(13) . ? F2 C57 1.323(12) . ? F3 C57 1.347(12) . ? S2 O12 1.401(11) . ? S2 O11 1.406(10) . ? S2 O10 1.422(9) . ? S2 C58 1.797(16) . ? F4 C58 1.36(2) . ? F5 C58 1.32(2) . ? F6 C58 1.301(19) . ? N9 C64 1.091(14) . ? C64 C63 1.481(16) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Mo1 O3 105.6(3) . . ? O2 Mo1 O1 106.2(3) . . ? O3 Mo1 O1 105.4(3) . . ? O2 Mo1 C23 103.3(3) . . ? O3 Mo1 C23 91.0(3) . . ? O1 Mo1 C23 140.6(3) . . ? O2 Mo1 C19 84.9(3) . . ? O3 Mo1 C19 124.9(3) . . ? O1 Mo1 C19 123.7(3) . . ? C23 Mo1 C19 35.0(3) . . ? O2 Mo1 C20 103.5(3) . . ? O3 Mo1 C20 140.6(3) . . ? O1 Mo1 C20 91.2(3) . . ? C23 Mo1 C20 56.5(3) . . ? C19 Mo1 C20 33.7(3) . . ? O2 Mo1 C22 137.2(3) . . ? O3 Mo1 C22 84.9(3) . . ? O1 Mo1 C22 110.7(3) . . ? C23 Mo1 C22 34.2(3) . . ? C19 Mo1 C22 56.9(3) . . ? C20 Mo1 C22 55.7(3) . . ? O2 Mo1 C21 137.0(3) . . ? O3 Mo1 C21 111.6(3) . . ? O1 Mo1 C21 84.1(3) . . ? C23 Mo1 C21 56.5(3) . . ? C19 Mo1 C21 56.6(3) . . ? C20 Mo1 C21 33.7(3) . . ? C22 Mo1 C21 33.4(3) . . ? O1 Co1 N3 100.3(3) . . ? O1 Co1 N1 102.9(3) . . ? N3 Co1 N1 116.4(3) . . ? O1 Co1 N4 104.9(3) . . ? N3 Co1 N4 114.1(3) . . ? N1 Co1 N4 115.4(3) . . ? O1 Co1 N2 177.5(3) . . ? N3 Co1 N2 77.4(3) . . ? N1 Co1 N2 77.2(3) . . ? N4 Co1 N2 77.2(3) . . ? Mo1 O1 Co1 147.1(3) . . ? C1 N1 C5 119.7(8) . . ? C1 N1 Co1 123.3(7) . . ? C5 N1 Co1 117.0(6) . . ? C7 N2 C6 112.3(7) . . ? C7 N2 C13 111.4(7) . . ? C6 N2 C13 111.1(7) . . ? C7 N2 Co1 107.5(6) . . ? C6 N2 Co1 106.9(5) . . ? C13 N2 Co1 107.3(5) . . ? C18 N3 C14 117.5(7) . . ? C18 N3 Co1 124.1(6) . . ? C14 N3 Co1 118.0(6) . . ? N1 C5 C4 121.9(9) . . ? N1 C5 C6 116.9(8) . . ? C4 C5 C6 121.2(9) . . ? N2 C6 C5 108.5(8) . . ? N2 C6 H6A 110.0 . . ? C5 C6 H6A 110.0 . . ? N2 C6 H6B 110.0 . . ? C5 C6 H6B 110.0 . . ? H6A C6 H6B 108.4 . . ? N2 C13 C14 110.5(7) . . ? N2 C13 H13A 109.5 . . ? C14 C13 H13A 109.5 . . ? N2 C13 H13B 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? N3 C14 C15 122.1(8) . . ? N3 C14 C13 116.2(8) . . ? C15 C14 C13 121.7(8) . . ? N3 C18 C17 124.4(8) . . ? N3 C18 H18 117.8 . . ? C17 C18 H18 117.8 . . ? C18 C17 C16 118.4(8) . . ? C18 C17 H17 120.8 . . ? C16 C17 H17 120.8 . . ? C15 C16 C17 117.8(8) . . ? C15 C16 H16 121.1 . . ? C17 C16 H16 121.1 . . ? C14 C15 C16 119.7(9) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? N2 C7 C8 109.6(7) . . ? N2 C7 H7A 109.8 . . ? C8 C7 H7A 109.8 . . ? N2 C7 H7B 109.8 . . ? C8 C7 H7B 109.8 . . ? H7A C7 H7B 108.2 . . ? N4 C8 C9 121.6(9) . . ? N4 C8 C7 115.2(8) . . ? C9 C8 C7 123.2(8) . . ? C12 N4 C8 118.9(8) . . ? C12 N4 Co1 123.8(6) . . ? C8 N4 Co1 117.2(6) . . ? N4 C12 C11 122.7(8) . . ? N4 C12 H12 118.6 . . ? C11 C12 H12 118.6 . . ? C12 C11 C10 118.0(9) . . ? C12 C11 H11 121.0 . . ? C10 C11 H11 121.0 . . ? C9 C10 C11 119.1(9) . . ? C9 C10 H10 120.4 . . ? C11 C10 H10 120.4 . . ? C10 C9 C8 119.6(9) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? C5 C4 C3 117.5(10) . . ? C5 C4 H4 121.3 . . ? C3 C4 H4 121.3 . . ? C2 C3 C4 119.7(10) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C3 C2 C1 119.7(11) . . ? C3 C2 H2 120.2 . . ? C1 C2 H2 120.2 . . ? N1 C1 C2 121.5(10) . . ? N1 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? C20 C19 C23 106.4(8) . . ? C20 C19 C24 127.0(8) . . ? C23 C19 C24 126.6(8) . . ? C20 C19 Mo1 74.0(5) . . ? C23 C19 Mo1 71.1(5) . . ? C24 C19 Mo1 121.5(6) . . ? C22 C23 C19 108.3(7) . . ? C22 C23 C28 125.1(8) . . ? C19 C23 C28 126.6(9) . . ? C22 C23 Mo1 75.7(5) . . ? C19 C23 Mo1 74.0(5) . . ? C28 C23 Mo1 117.9(6) . . ? C21 C22 C23 108.4(8) . . ? C21 C22 C27 127.6(8) . . ? C23 C22 C27 124.0(8) . . ? C21 C22 Mo1 74.4(5) . . ? C23 C22 Mo1 70.1(5) . . ? C27 C22 Mo1 120.8(6) . . ? C22 C21 C20 106.9(8) . . ? C22 C21 C26 125.8(8) . . ? C20 C21 C26 127.3(8) . . ? C22 C21 Mo1 72.2(5) . . ? C20 C21 Mo1 71.6(5) . . ? C26 C21 Mo1 121.0(6) . . ? C19 C20 C21 110.0(7) . . ? C19 C20 C25 124.7(8) . . ? C21 C20 C25 125.3(8) . . ? C19 C20 Mo1 72.3(5) . . ? C21 C20 Mo1 74.7(5) . . ? C25 C20 Mo1 122.3(5) . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O6 Mo2 O5 105.7(3) . . ? O6 Mo2 O4 104.9(3) . . ? O5 Mo2 O4 106.3(3) . . ? O6 Mo2 C49 90.5(3) . . ? O5 Mo2 C49 102.3(3) . . ? O4 Mo2 C49 142.1(3) . . ? O6 Mo2 C48 124.6(3) . . ? O5 Mo2 C48 84.9(3) . . ? O4 Mo2 C48 124.3(3) . . ? C49 Mo2 C48 34.9(3) . . ? O6 Mo2 C50 83.8(3) . . ? O5 Mo2 C50 136.5(3) . . ? O4 Mo2 C50 112.0(3) . . ? C49 Mo2 C50 34.3(3) . . ? C48 Mo2 C50 56.8(3) . . ? O6 Mo2 C47 139.5(3) . . ? O5 Mo2 C47 104.1(3) . . ? O4 Mo2 C47 92.2(3) . . ? C49 Mo2 C47 56.5(3) . . ? C48 Mo2 C47 33.6(3) . . ? C50 Mo2 C47 55.7(3) . . ? O6 Mo2 C51 110.3(3) . . ? O5 Mo2 C51 137.4(3) . . ? O4 Mo2 C51 85.7(3) . . ? C49 Mo2 C51 56.3(3) . . ? C48 Mo2 C51 56.2(3) . . ? C50 Mo2 C51 33.1(3) . . ? C47 Mo2 C51 33.6(3) . . ? O4 Co2 N5 103.4(3) . . ? O4 Co2 N8 99.8(3) . . ? N5 Co2 N8 118.4(3) . . ? O4 Co2 N7 105.5(3) . . ? N5 Co2 N7 111.9(3) . . ? N8 Co2 N7 115.3(3) . . ? O4 Co2 N6 176.6(3) . . ? N5 Co2 N6 76.7(3) . . ? N8 Co2 N6 77.3(3) . . ? N7 Co2 N6 77.4(3) . . ? Mo2 O4 Co2 148.4(3) . . ? C34 N6 C41 113.2(7) . . ? C34 N6 C35 112.8(7) . . ? C41 N6 C35 110.3(7) . . ? C34 N6 Co2 105.3(5) . . ? C41 N6 Co2 107.2(5) . . ? C35 N6 Co2 107.6(5) . . ? N6 C35 C36 110.1(7) . . ? N6 C35 H35A 109.6 . . ? C36 C35 H35A 109.6 . . ? N6 C35 H35B 109.6 . . ? C36 C35 H35B 109.6 . . ? H35A C35 H35B 108.1 . . ? N7 C36 C37 122.0(8) . . ? N7 C36 C35 116.1(7) . . ? C37 C36 C35 121.9(8) . . ? C40 N7 C36 118.7(7) . . ? C40 N7 Co2 123.8(6) . . ? C36 N7 Co2 117.5(6) . . ? N7 C40 C39 122.9(8) . . ? N7 C40 H40 118.5 . . ? C39 C40 H40 118.5 . . ? C40 C39 C38 118.6(8) . . ? C40 C39 H39 120.7 . . ? C38 C39 H39 120.7 . . ? C39 C38 C37 119.0(8) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C36 C37 C38 118.7(8) . . ? C36 C37 H37 120.7 . . ? C38 C37 H37 120.7 . . ? N6 C34 C33 110.5(7) . . ? N6 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? N6 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? N5 C33 C32 122.1(8) . . ? N5 C33 C34 114.4(8) . . ? C32 C33 C34 123.5(8) . . ? C33 N5 C29 118.4(7) . . ? C33 N5 Co2 117.6(6) . . ? C29 N5 Co2 123.9(6) . . ? C30 C29 N5 120.9(9) . . ? C30 C29 H29 119.6 . . ? N5 C29 H29 119.6 . . ? C29 C30 C31 120.7(9) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C32 C31 C30 119.2(9) . . ? C32 C31 H31 120.4 . . ? C30 C31 H31 120.4 . . ? C31 C32 C33 118.7(9) . . ? C31 C32 H32 120.7 . . ? C33 C32 H32 120.7 . . ? N6 C41 C42 111.0(7) . . ? N6 C41 H41A 109.4 . . ? C42 C41 H41A 109.4 . . ? N6 C41 H41B 109.4 . . ? C42 C41 H41B 109.4 . . ? H41A C41 H41B 108.0 . . ? N8 C42 C43 121.4(8) . . ? N8 C42 C41 116.1(8) . . ? C43 C42 C41 122.5(8) . . ? C42 N8 C46 119.3(7) . . ? C42 N8 Co2 117.4(6) . . ? C46 N8 Co2 123.0(6) . . ? N8 C46 C45 121.6(9) . . ? N8 C46 H46 119.2 . . ? C45 C46 H46 119.2 . . ? C44 C45 C46 119.5(9) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? C45 C44 C43 119.0(9) . . ? C45 C44 H44 120.5 . . ? C43 C44 H44 120.5 . . ? C42 C43 C44 119.1(9) . . ? C42 C43 H43 120.4 . . ? C44 C43 H43 120.4 . . ? C48 C47 C51 108.9(7) . . ? C48 C47 C53 125.5(8) . . ? C51 C47 C53 125.5(8) . . ? C48 C47 Mo2 72.0(5) . . ? C51 C47 Mo2 73.8(4) . . ? C53 C47 Mo2 122.5(5) . . ? C47 C48 C49 107.0(8) . . ? C47 C48 C54 126.9(8) . . ? C49 C48 C54 126.1(9) . . ? C47 C48 Mo2 74.4(5) . . ? C49 C48 Mo2 70.9(4) . . ? C54 C48 Mo2 121.8(6) . . ? C50 C49 C48 107.7(7) . . ? C50 C49 C55 126.2(8) . . ? C48 C49 C55 126.0(8) . . ? C50 C49 Mo2 75.2(5) . . ? C48 C49 Mo2 74.1(5) . . ? C55 C49 Mo2 118.5(5) . . ? C51 C50 C49 108.3(7) . . ? C51 C50 C56 127.1(8) . . ? C49 C50 C56 124.6(8) . . ? C51 C50 Mo2 74.5(4) . . ? C49 C50 Mo2 70.4(4) . . ? C56 C50 Mo2 121.5(6) . . ? C50 C51 C47 108.1(8) . . ? C50 C51 C52 125.6(8) . . ? C47 C51 C52 126.3(7) . . ? C50 C51 Mo2 72.4(5) . . ? C47 C51 Mo2 72.6(4) . . ? C52 C51 Mo2 121.0(5) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C56 H56A 109.5 . . ? C50 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C50 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C49 C55 H55A 109.5 . . ? C49 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C49 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C48 C54 H54A 109.5 . . ? C48 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C48 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C47 C53 H53A 109.5 . . ? C47 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C47 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C60 O13 C61 117.2(15) . . ? C60 C59 H59A 109.5 . . ? C60 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C60 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? O13 C60 C59 109.4(18) . . ? O13 C60 H60A 109.8 . . ? C59 C60 H60A 109.8 . . ? O13 C60 H60B 109.8 . . ? C59 C60 H60B 109.8 . . ? H60A C60 H60B 108.2 . . ? O13 C61 C62 111.1(18) . . ? O13 C61 H61A 109.4 . . ? C62 C61 H61A 109.4 . . ? O13 C61 H61B 109.4 . . ? C62 C61 H61B 109.4 . . ? H61A C61 H61B 108.0 . . ? 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 . . ? O9 S1 O7 115.6(5) . . ? O9 S1 O8 115.4(5) . . ? O7 S1 O8 113.5(5) . . ? O9 S1 C57 102.9(5) . . ? O7 S1 C57 103.3(5) . . ? O8 S1 C57 103.9(5) . . ? F2 C57 F3 107.7(8) . . ? F2 C57 F1 107.5(9) . . ? F3 C57 F1 106.7(9) . . ? F2 C57 S1 112.8(7) . . ? F3 C57 S1 111.3(7) . . ? F1 C57 S1 110.4(7) . . ? O12 S2 O11 115.7(10) . . ? O12 S2 O10 115.5(9) . . ? O11 S2 O10 112.8(7) . . ? O12 S2 C58 104.3(9) . . ? O11 S2 C58 102.9(9) . . ? O10 S2 C58 103.3(7) . . ? F6 C58 F5 109.9(18) . . ? F6 C58 F4 107.1(15) . . ? F5 C58 F4 102.0(17) . . ? F6 C58 S2 114.1(13) . . ? F5 C58 S2 112.9(12) . . ? F4 C58 S2 109.9(14) . . ? N9 C64 C63 177.5(14) . . ? C64 C63 H63A 109.5 . . ? C64 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C64 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 2.590 _refine_diff_density_min -1.507 _refine_diff_density_rms 0.169 _database_code_depnum_ccdc_archive 'CCDC 936997' ####################################################################### # # 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_c:2012_jf184 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H36 Co2 Mo2 N8 O8, 2(C4 H6 N2), 2(C F3 O3 S)' _chemical_formula_sum 'C46 H48 Co2 F6 Mo2 N12 O14 S2' _chemical_formula_weight 1480.82 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.080(5) _cell_length_b 15.135(3) _cell_length_c 16.790(3) _cell_angle_alpha 90.00 _cell_angle_beta 116.26(3) _cell_angle_gamma 90.00 _cell_volume 5488(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 738 _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 16.66 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.792 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2976 _exptl_absorpt_coefficient_mu 1.213 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'STOE X-RED' _exptl_absorpt_correction_T_min 0.8047 _exptl_absorpt_correction_T_max 0.8994 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 1 1 -1 0.0710 -1 -1 1 0.0680 -7 2 3 0.0620 7 -2 -3 0.1010 7 1 -4 0.0760 1 0 0 0.0610 -1 0 0 0.0410 3 -2 -5 0.0800 -3 2 5 0.0880 _exptl_special_details ; ? ; _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 45 _diffrn_source_power 2.25 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 100(2) _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_ambient_temperature 100(2) _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 436 frames, detector distance = 110 mm ; _diffrn_reflns_number 46109 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_av_unetI/netI 0.1604 _diffrn_reflns_av_R_equivalents 0.1093 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _reflns_d_resolution_high 0.811 _reflns_d_resolution_low 6.331 _reflns_special_details 'Friedel pairs have been merged' _reflns_limit_h_min -29 _reflns_limit_h_max 26 _reflns_limit_k_min 0 _reflns_limit_k_max 18 _reflns_limit_l_min 0 _reflns_limit_l_max 20 _reflns_number_total 5399 _reflns_number_gt 2911 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution SIR97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0526P)^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 5399 _refine_ls_number_parameters 425 _refine_ls_number_restraints 84 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1326 _refine_ls_wR_factor_gt 0.1289 _refine_ls_goodness_of_fit_ref 0.877 _refine_ls_restrained_S_all 0.871 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.275 _refine_diff_density_min -0.948 _refine_diff_density_rms 0.135 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 Co1 Co 0.26651(5) 0.61119(7) 0.38548(6) 0.0145(2) Uani 1 1 d . . . Mo1 Mo 0.17903(3) 0.72547(4) 0.42314(4) 0.01284(16) Uani 1 1 d . . . C1 C 0.3608(4) 0.5028(6) 0.3785(5) 0.0237(19) Uani 1 1 d . . . H1A H 0.3727 0.4446 0.4082 0.028 Uiso 1 1 calc R . . H1B H 0.3951 0.5238 0.3662 0.028 Uiso 1 1 calc R . . C2 C 0.3028(4) 0.4925(5) 0.2917(5) 0.0175(17) Uani 1 1 d . . . C3 C 0.3006(4) 0.4414(5) 0.2226(5) 0.0224(18) Uani 1 1 d . . . H3 H 0.3365 0.4119 0.2265 0.027 Uiso 1 1 calc R . . C4 C 0.2452(4) 0.4339(5) 0.1479(5) 0.0211(18) Uani 1 1 d . . . H4 H 0.2424 0.3978 0.1001 0.025 Uiso 1 1 calc R . . C5 C 0.1932(4) 0.4786(5) 0.1418(5) 0.0220(18) Uani 1 1 d . . . H5 H 0.1551 0.4748 0.0895 0.026 Uiso 1 1 calc R . . C6 C 0.1979(4) 0.5291(5) 0.2134(5) 0.0206(18) Uani 1 1 d . . . H6 H 0.1624 0.5584 0.2114 0.025 Uiso 1 1 calc R . . C7 C 0.3589(4) 0.5199(5) 0.5242(5) 0.0214(18) Uani 1 1 d . . . H7A H 0.3930 0.4762 0.5424 0.026 Uiso 1 1 calc R . . H7B H 0.3690 0.5630 0.5729 0.026 Uiso 1 1 calc R . . C8 C 0.3001(4) 0.4753(5) 0.5049(5) 0.0199(17) Uani 1 1 d . . . C9 C 0.2939(4) 0.3978(5) 0.5475(5) 0.027(2) Uani 1 1 d . . . H9 H 0.3299 0.3700 0.5911 0.032 Uiso 1 1 calc R . . C10 C 0.2379(4) 0.3632(5) 0.5272(5) 0.028(2) Uani 1 1 d . . . H10 H 0.2342 0.3111 0.5561 0.034 Uiso 1 1 calc R . . C11 C 0.1850(4) 0.4041(5) 0.4632(6) 0.028(2) Uani 1 1 d . . . H11 H 0.1449 0.3813 0.4486 0.033 Uiso 1 1 calc R . . C12 C 0.1927(4) 0.4784(5) 0.4220(5) 0.0184(18) Uani 1 1 d . . . H12 H 0.1573 0.5057 0.3766 0.022 Uiso 1 1 calc R . . C13 C 0.3915(3) 0.6448(5) 0.4541(5) 0.0219(18) Uani 1 1 d . . . H13A H 0.4326 0.6261 0.4605 0.026 Uiso 1 1 calc R . . H13B H 0.3972 0.6758 0.5091 0.026 Uiso 1 1 calc R . . C14 C 0.3610(3) 0.7055(5) 0.3751(5) 0.0160(16) Uani 1 1 d U . . C15 C 0.3919(4) 0.7607(6) 0.3433(5) 0.030(2) Uani 1 1 d . . . H15 H 0.4357 0.7650 0.3730 0.036 Uiso 1 1 calc R . . C16 C 0.3580(4) 0.8108(6) 0.2666(6) 0.032(2) Uani 1 1 d . . . H16 H 0.3778 0.8520 0.2450 0.038 Uiso 1 1 calc R . . C17 C 0.2953(4) 0.7978(5) 0.2241(5) 0.028(2) Uani 1 1 d . . . H17 H 0.2718 0.8263 0.1688 0.033 Uiso 1 1 calc R . . C18 C 0.2656(3) 0.7447(5) 0.2592(5) 0.0180(17) Uani 1 1 d . . . H18 H 0.2218 0.7402 0.2310 0.022 Uiso 1 1 calc R . . N1 N 0.3511(3) 0.5670(4) 0.4395(4) 0.0162(14) Uani 1 1 d U . . N2 N 0.2527(3) 0.5367(4) 0.2860(4) 0.0159(14) Uani 1 1 d . . . N3 N 0.2485(3) 0.5132(4) 0.4440(4) 0.0198(15) Uani 1 1 d . . . N4 N 0.2994(3) 0.6990(4) 0.3343(4) 0.0179(14) Uani 1 1 d . . . O1 O 0.1859(2) 0.6576(3) 0.3363(3) 0.0169(11) Uani 1 1 d . . . O2 O 0.2729(2) 0.6904(3) 0.4790(3) 0.0143(11) Uani 1 1 d . . . O3 O 0.1282(2) 0.8049(3) 0.3585(3) 0.0206(12) Uani 1 1 d . . . O4 O 0.1406(2) 0.6618(3) 0.4670(3) 0.0198(12) Uani 1 1 d . . . N200 N 0.4288(7) 0.5339(11) 0.2519(10) 0.031(3) Uani 0.50 1 d PU A 1 C201 C 0.4610(8) 0.4815(12) 0.2457(11) 0.029(4) Uani 0.50 1 d PU A 1 C202 C 0.5000 0.4128(12) 0.2500 0.072(5) Uani 1 2 d SU A 1 H20A H 0.5306 0.4039 0.3118 0.108 Uiso 0.50 1 calc PR A 1 H20B H 0.5214 0.4271 0.2137 0.108 Uiso 0.50 1 calc PR A 1 H20C H 0.4757 0.3587 0.2275 0.108 Uiso 0.50 1 calc PR A 1 N210 N 0.4207(7) 0.5953(11) 0.2405(10) 0.036(4) Uani 0.50 1 d PU B 2 C211 C 0.4552(8) 0.6506(12) 0.2451(11) 0.028(4) Uani 0.50 1 d PU B 2 C212 C 0.5000 0.7221(10) 0.2500 0.043(3) Uani 1 2 d SU B 2 H21A H 0.5412 0.6964 0.2685 0.065 Uiso 0.50 1 calc PR B 2 H21B H 0.5018 0.7669 0.2932 0.065 Uiso 0.50 1 calc PR B 2 H21C H 0.4862 0.7496 0.1915 0.065 Uiso 0.50 1 calc PR B 2 N300 N 0.4480(8) -0.0266(12) 0.3322(13) 0.051(5) Uani 0.50 1 d PU C 1 C301 C 0.4800(10) -0.0082(15) 0.3985(15) 0.050(5) Uani 0.50 1 d PU C 1 C302 C 0.5241(10) 0.0155(16) 0.4879(16) 0.059(6) Uani 0.50 1 d PU C 1 H30A H 0.5428 -0.0382 0.5217 0.089 Uiso 0.50 1 calc PR C 1 H30B H 0.5028 0.0478 0.5168 0.089 Uiso 0.50 1 calc PR C 1 H30C H 0.5565 0.0529 0.4855 0.089 Uiso 0.50 1 calc PR C 1 N310 N 0.4462(8) -0.0101(12) 0.2723(12) 0.047(4) Uani 0.50 1 d PU D 2 C311 C 0.4714(9) 0.0523(14) 0.2709(14) 0.043(5) Uani 0.50 1 d PU D 2 C312 C 0.5000 0.1309(11) 0.2500 0.063(5) Uani 1 2 d SU D 2 H31A H 0.5265 0.1114 0.2227 0.094 Uiso 0.50 1 calc PR D 2 H31B H 0.5250 0.1633 0.3048 0.094 Uiso 0.50 1 calc PR D 2 H31C H 0.4673 0.1696 0.2087 0.094 Uiso 0.50 1 calc PR D 2 F101 F 0.5031(2) 0.2273(4) 0.4344(3) 0.0421(13) Uani 1 1 d . . . F102 F 0.4119(3) 0.1808(5) 0.3533(5) 0.076(2) Uani 1 1 d . . . F103 F 0.4337(3) 0.3166(5) 0.3475(4) 0.076(2) Uani 1 1 d . . . C100 C 0.4431(4) 0.2484(6) 0.4010(6) 0.036(2) Uani 1 1 d . . . S100 S 0.42028(9) 0.27454(16) 0.48768(13) 0.0252(4) Uani 1 1 d . . . O101 O 0.3556(2) 0.2904(4) 0.4384(4) 0.0338(15) Uani 1 1 d . . . O102 O 0.4564(3) 0.3514(4) 0.5278(4) 0.0363(16) Uani 1 1 d . . . O103 O 0.4376(3) 0.1956(4) 0.5428(4) 0.0460(19) 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 Co1 0.0196(6) 0.0159(5) 0.0078(5) -0.0010(4) 0.0058(4) 0.0007(4) Mo1 0.0149(3) 0.0153(3) 0.0068(3) -0.0005(3) 0.0034(2) -0.0001(3) C1 0.025(4) 0.026(5) 0.021(4) -0.006(3) 0.011(4) 0.009(4) C2 0.025(4) 0.017(4) 0.012(4) -0.001(3) 0.010(3) 0.003(3) C3 0.032(5) 0.019(4) 0.019(4) 0.001(3) 0.014(4) -0.002(4) C4 0.032(5) 0.023(4) 0.009(4) -0.006(3) 0.009(3) -0.008(4) C5 0.029(5) 0.020(4) 0.013(4) -0.004(3) 0.006(3) 0.000(4) C6 0.024(4) 0.019(4) 0.014(4) -0.007(3) 0.005(3) 0.000(3) C7 0.032(5) 0.021(4) 0.009(4) 0.001(3) 0.007(3) 0.007(4) C8 0.028(5) 0.024(4) 0.010(4) -0.002(3) 0.010(3) 0.005(4) C9 0.055(6) 0.014(4) 0.022(4) 0.009(3) 0.027(4) 0.012(4) C10 0.054(6) 0.018(4) 0.025(5) 0.001(4) 0.028(4) 0.003(4) C11 0.041(5) 0.018(4) 0.033(5) -0.009(4) 0.025(4) -0.007(4) C12 0.023(5) 0.018(4) 0.013(4) -0.006(3) 0.007(3) -0.006(3) C13 0.015(4) 0.040(5) 0.007(3) -0.001(3) 0.001(3) 0.005(4) C14 0.019(3) 0.019(3) 0.014(3) -0.001(2) 0.010(2) -0.001(2) C15 0.027(4) 0.045(6) 0.023(4) -0.001(4) 0.016(4) -0.011(4) C16 0.038(5) 0.031(5) 0.035(5) -0.005(4) 0.024(5) -0.008(4) C17 0.044(5) 0.021(5) 0.013(4) -0.002(3) 0.008(4) -0.010(4) C18 0.021(4) 0.018(4) 0.016(4) -0.004(3) 0.009(3) -0.002(3) N1 0.021(2) 0.018(2) 0.011(2) -0.0002(19) 0.0089(19) 0.002(2) N2 0.019(3) 0.011(3) 0.014(3) 0.002(3) 0.004(3) 0.002(3) N3 0.028(4) 0.022(4) 0.015(3) -0.007(3) 0.014(3) 0.001(3) N4 0.023(4) 0.017(3) 0.014(3) -0.002(2) 0.008(3) 0.003(3) O1 0.015(3) 0.026(3) 0.005(2) -0.004(2) 0.001(2) -0.002(2) O2 0.011(3) 0.022(3) 0.009(2) -0.002(2) 0.003(2) 0.003(2) O3 0.025(3) 0.025(3) 0.008(2) -0.001(2) 0.004(2) 0.003(2) O4 0.021(3) 0.022(3) 0.019(3) -0.001(2) 0.012(2) -0.004(2) N200 0.031(4) 0.033(4) 0.031(4) 0.001(3) 0.016(3) -0.002(3) C201 0.029(5) 0.029(5) 0.028(5) 0.001(3) 0.012(3) 0.000(3) C202 0.070(6) 0.070(6) 0.075(6) 0.000 0.030(3) 0.000 N210 0.035(4) 0.037(5) 0.035(4) -0.001(3) 0.015(3) 0.001(3) C211 0.028(5) 0.028(5) 0.027(5) 0.000(3) 0.012(3) 0.002(3) C212 0.045(4) 0.044(4) 0.041(4) 0.000 0.020(3) 0.000 N300 0.050(5) 0.050(5) 0.052(5) 0.001(3) 0.022(3) -0.002(3) C301 0.050(6) 0.049(6) 0.050(6) 0.000(3) 0.022(4) 0.000(3) C302 0.059(7) 0.058(7) 0.059(7) 0.000(3) 0.025(4) 0.000(3) N310 0.046(5) 0.046(5) 0.046(5) -0.001(3) 0.018(3) -0.001(3) C311 0.044(6) 0.043(6) 0.041(6) -0.001(3) 0.019(3) -0.001(3) C312 0.063(5) 0.062(5) 0.064(5) 0.000 0.028(3) 0.000 F101 0.021(2) 0.055(3) 0.052(3) -0.023(3) 0.017(2) -0.001(3) F102 0.042(4) 0.098(6) 0.081(5) -0.063(4) 0.022(3) -0.014(4) F103 0.094(5) 0.114(6) 0.032(3) 0.023(4) 0.040(4) 0.029(5) C100 0.028(5) 0.040(6) 0.027(5) -0.016(4) 0.000(4) -0.009(4) S100 0.0240(10) 0.0266(11) 0.0244(10) 0.0040(10) 0.0101(8) 0.0022(10) O101 0.020(3) 0.038(4) 0.039(3) 0.003(3) 0.009(3) 0.004(3) O102 0.032(4) 0.029(3) 0.040(4) -0.005(3) 0.008(3) 0.001(3) O103 0.045(4) 0.041(4) 0.044(4) 0.024(3) 0.013(3) 0.003(3) _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 Co1 O1 1.877(5) . ? Co1 N2 1.918(6) . ? Co1 O2 1.927(5) . ? Co1 N3 1.931(7) . ? Co1 N4 1.932(6) . ? Co1 N1 1.944(6) . ? Co1 Mo1 3.0013(13) . ? Mo1 O4 1.712(5) . ? Mo1 O3 1.717(5) . ? Mo1 O1 1.850(5) . ? Mo1 O2 1.994(5) 7_566 ? Mo1 O2 2.096(5) . ? C1 N1 1.502(9) . ? C1 C2 1.516(11) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.346(9) . ? C2 C3 1.375(11) . ? C3 C4 1.372(11) . ? C3 H3 0.9500 . ? C4 C5 1.385(11) . ? C4 H4 0.9500 . ? C5 C6 1.387(10) . ? C5 H5 0.9500 . ? C6 N2 1.348(9) . ? C6 H6 0.9500 . ? C7 C8 1.470(11) . ? C7 N1 1.526(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N3 1.341(10) . ? C8 C9 1.415(11) . ? C9 C10 1.344(12) . ? C9 H9 0.9500 . ? C10 C11 1.396(12) . ? C10 H10 0.9500 . ? C11 C12 1.374(11) . ? C11 H11 0.9500 . ? C12 N3 1.335(9) . ? C12 H12 0.9500 . ? C13 N1 1.477(10) . ? C13 C14 1.510(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N4 1.334(9) . ? C14 C15 1.375(11) . ? C15 C16 1.403(12) . ? C15 H15 0.9500 . ? C16 C17 1.369(12) . ? C16 H16 0.9500 . ? C17 C18 1.370(10) . ? C17 H17 0.9500 . ? C18 N4 1.350(9) . ? C18 H18 0.9500 . ? O2 Mo1 1.994(5) 7_566 ? N200 C201 1.15(2) . ? C201 C202 1.38(2) . ? C202 H20A 0.9800 . ? C202 H20B 0.9800 . ? C202 H20C 0.9800 . ? N210 C211 1.16(2) . ? C211 C212 1.50(2) . ? C212 H21A 0.9800 . ? C212 H21B 0.9800 . ? C212 H21C 0.9800 . ? N300 C301 1.07(2) . ? C301 C302 1.45(3) . ? C302 H30A 0.9800 . ? C302 H30B 0.9800 . ? C302 H30C 0.9800 . ? N310 C311 1.13(2) . ? C311 C312 1.49(2) . ? C312 H31A 0.9800 . ? C312 H31B 0.9800 . ? C312 H31C 0.9800 . ? F101 C100 1.338(10) . ? F102 C100 1.312(10) . ? F103 C100 1.320(11) . ? C100 S100 1.811(10) . ? S100 O101 1.424(6) . ? S100 O102 1.431(6) . ? S100 O103 1.454(6) . ? 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 O1 Co1 N2 95.2(2) . . ? O1 Co1 O2 79.6(2) . . ? N2 Co1 O2 174.8(2) . . ? O1 Co1 N3 95.1(3) . . ? N2 Co1 N3 90.0(3) . . ? O2 Co1 N3 91.0(2) . . ? O1 Co1 N4 95.4(2) . . ? N2 Co1 N4 88.0(3) . . ? O2 Co1 N4 91.9(2) . . ? N3 Co1 N4 169.4(3) . . ? O1 Co1 N1 177.8(2) . . ? N2 Co1 N1 86.9(3) . . ? O2 Co1 N1 98.3(2) . . ? N3 Co1 N1 85.6(3) . . ? N4 Co1 N1 83.9(3) . . ? O1 Co1 Mo1 36.05(14) . . ? N2 Co1 Mo1 130.91(19) . . ? O2 Co1 Mo1 43.96(14) . . ? N3 Co1 Mo1 89.90(19) . . ? N4 Co1 Mo1 99.24(18) . . ? N1 Co1 Mo1 141.98(18) . . ? O4 Mo1 O3 107.2(3) . . ? O4 Mo1 O1 106.3(2) . . ? O3 Mo1 O1 100.3(2) . . ? O4 Mo1 O2 103.4(2) . 7_566 ? O3 Mo1 O2 93.7(2) . 7_566 ? O1 Mo1 O2 141.4(2) . 7_566 ? O4 Mo1 O2 110.2(2) . . ? O3 Mo1 O2 141.9(2) . . ? O1 Mo1 O2 75.9(2) . . ? O2 Mo1 O2 71.1(2) 7_566 . ? O4 Mo1 Co1 109.22(18) . . ? O3 Mo1 Co1 129.91(18) . . ? O1 Mo1 Co1 36.66(15) . . ? O2 Mo1 Co1 109.63(14) 7_566 . ? O2 Mo1 Co1 39.65(13) . . ? N1 C1 C2 111.5(6) . . ? N1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? N1 C1 H1B 109.3 . . ? C2 C1 H1B 109.3 . . ? H1A C1 H1B 108.0 . . ? N2 C2 C3 121.4(7) . . ? N2 C2 C1 115.6(6) . . ? C3 C2 C1 123.1(7) . . ? C4 C3 C2 118.5(8) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 120.6(7) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C4 C5 C6 118.7(7) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? N2 C6 C5 120.2(8) . . ? N2 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C8 C7 N1 107.4(6) . . ? C8 C7 H7A 110.2 . . ? N1 C7 H7A 110.2 . . ? C8 C7 H7B 110.2 . . ? N1 C7 H7B 110.2 . . ? H7A C7 H7B 108.5 . . ? N3 C8 C9 118.1(8) . . ? N3 C8 C7 116.7(7) . . ? C9 C8 C7 125.2(7) . . ? C10 C9 C8 120.9(8) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 119.6(8) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C12 C11 C10 118.1(8) . . ? C12 C11 H11 121.0 . . ? C10 C11 H11 121.0 . . ? N3 C12 C11 121.8(8) . . ? N3 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? N1 C13 C14 108.0(6) . . ? N1 C13 H13A 110.1 . . ? C14 C13 H13A 110.1 . . ? N1 C13 H13B 110.1 . . ? C14 C13 H13B 110.1 . . ? H13A C13 H13B 108.4 . . ? N4 C14 C15 121.0(7) . . ? N4 C14 C13 113.9(6) . . ? C15 C14 C13 125.1(7) . . ? C14 C15 C16 119.4(8) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C17 C16 C15 117.4(8) . . ? C17 C16 H16 121.3 . . ? C15 C16 H16 121.3 . . ? C16 C17 C18 121.6(8) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? N4 C18 C17 119.3(7) . . ? N4 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C13 N1 C1 109.8(6) . . ? C13 N1 C7 114.6(6) . . ? C1 N1 C7 109.9(6) . . ? C13 N1 Co1 106.3(5) . . ? C1 N1 Co1 110.6(5) . . ? C7 N1 Co1 105.5(5) . . ? C2 N2 C6 120.6(6) . . ? C2 N2 Co1 115.2(5) . . ? C6 N2 Co1 124.1(5) . . ? C12 N3 C8 121.5(7) . . ? C12 N3 Co1 126.0(5) . . ? C8 N3 Co1 112.0(5) . . ? C14 N4 C18 121.0(7) . . ? C14 N4 Co1 113.7(5) . . ? C18 N4 Co1 124.9(5) . . ? Mo1 O1 Co1 107.3(2) . . ? Co1 O2 Mo1 151.2(3) . 7_566 ? Co1 O2 Mo1 96.4(2) . . ? Mo1 O2 Mo1 108.9(2) 7_566 . ? N200 C201 C202 171.2(18) . . ? N210 C211 C212 179.3(18) . . ? C211 C212 H21A 109.5 . . ? C211 C212 H21B 109.5 . . ? H21A C212 H21B 109.5 . . ? C211 C212 H21C 109.5 . . ? H21A C212 H21C 109.5 . . ? H21B C212 H21C 109.5 . . ? N300 C301 C302 179(3) . . ? N310 C311 C312 169(2) . . ? C311 C312 H31A 109.5 . . ? C311 C312 H31B 109.5 . . ? H31A C312 H31B 109.5 . . ? C311 C312 H31C 109.5 . . ? H31A C312 H31C 109.5 . . ? H31B C312 H31C 109.5 . . ? F102 C100 F103 108.4(8) . . ? F102 C100 F101 106.8(7) . . ? F103 C100 F101 107.4(8) . . ? F102 C100 S100 111.5(7) . . ? F103 C100 S100 110.8(6) . . ? F101 C100 S100 111.8(6) . . ? O101 S100 O102 114.7(4) . . ? O101 S100 O103 116.1(4) . . ? O102 S100 O103 115.1(4) . . ? O101 S100 C100 102.3(4) . . ? O102 S100 C100 102.6(4) . . ? O103 S100 C100 103.2(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Co1 Mo1 O4 91.6(3) . . . . ? N2 Co1 Mo1 O4 82.7(3) . . . . ? O2 Co1 Mo1 O4 -98.8(3) . . . . ? N3 Co1 Mo1 O4 -7.2(3) . . . . ? N4 Co1 Mo1 O4 178.1(3) . . . . ? N1 Co1 Mo1 O4 -90.0(4) . . . . ? O1 Co1 Mo1 O3 -42.9(4) . . . . ? N2 Co1 Mo1 O3 -51.7(3) . . . . ? O2 Co1 Mo1 O3 126.8(3) . . . . ? N3 Co1 Mo1 O3 -141.7(3) . . . . ? N4 Co1 Mo1 O3 43.6(3) . . . . ? N1 Co1 Mo1 O3 135.5(4) . . . . ? N2 Co1 Mo1 O1 -8.9(4) . . . . ? O2 Co1 Mo1 O1 169.6(4) . . . . ? N3 Co1 Mo1 O1 -98.8(3) . . . . ? N4 Co1 Mo1 O1 86.5(3) . . . . ? N1 Co1 Mo1 O1 178.4(4) . . . . ? O1 Co1 Mo1 O2 -155.7(3) . . . 7_566 ? N2 Co1 Mo1 O2 -164.6(3) . . . 7_566 ? O2 Co1 Mo1 O2 13.9(4) . . . 7_566 ? N3 Co1 Mo1 O2 105.5(2) . . . 7_566 ? N4 Co1 Mo1 O2 -69.2(2) . . . 7_566 ? N1 Co1 Mo1 O2 22.7(3) . . . 7_566 ? O1 Co1 Mo1 O2 -169.6(4) . . . . ? N2 Co1 Mo1 O2 -178.5(3) . . . . ? N3 Co1 Mo1 O2 91.5(3) . . . . ? N4 Co1 Mo1 O2 -83.1(3) . . . . ? N1 Co1 Mo1 O2 8.8(4) . . . . ? N1 C1 C2 N2 -4.1(10) . . . . ? N1 C1 C2 C3 176.3(8) . . . . ? N2 C2 C3 C4 -2.0(12) . . . . ? C1 C2 C3 C4 177.7(7) . . . . ? C2 C3 C4 C5 1.5(12) . . . . ? C3 C4 C5 C6 -1.7(12) . . . . ? C4 C5 C6 N2 2.4(12) . . . . ? N1 C7 C8 N3 -30.3(9) . . . . ? N1 C7 C8 C9 152.0(7) . . . . ? N3 C8 C9 C10 0.4(11) . . . . ? C7 C8 C9 C10 178.0(7) . . . . ? C8 C9 C10 C11 -0.1(12) . . . . ? C9 C10 C11 C12 1.1(11) . . . . ? C10 C11 C12 N3 -2.5(11) . . . . ? N1 C13 C14 N4 27.6(8) . . . . ? N1 C13 C14 C15 -149.7(7) . . . . ? N4 C14 C15 C16 -0.2(12) . . . . ? C13 C14 C15 C16 176.9(7) . . . . ? C14 C15 C16 C17 -3.7(12) . . . . ? C15 C16 C17 C18 6.2(12) . . . . ? C16 C17 C18 N4 -4.8(12) . . . . ? C14 C13 N1 C1 80.5(7) . . . . ? C14 C13 N1 C7 -155.3(6) . . . . ? C14 C13 N1 Co1 -39.2(6) . . . . ? C2 C1 N1 C13 -115.4(7) . . . . ? C2 C1 N1 C7 117.7(7) . . . . ? C2 C1 N1 Co1 1.5(8) . . . . ? C8 C7 N1 C13 153.7(6) . . . . ? C8 C7 N1 C1 -82.1(7) . . . . ? C8 C7 N1 Co1 37.1(6) . . . . ? N2 Co1 N1 C13 119.8(5) . . . . ? O2 Co1 N1 C13 -59.6(4) . . . . ? N3 Co1 N1 C13 -149.9(5) . . . . ? N4 Co1 N1 C13 31.5(4) . . . . ? Mo1 Co1 N1 C13 -65.7(5) . . . . ? N2 Co1 N1 C1 0.6(5) . . . . ? O2 Co1 N1 C1 -178.7(5) . . . . ? N3 Co1 N1 C1 90.9(5) . . . . ? N4 Co1 N1 C1 -87.6(5) . . . . ? Mo1 Co1 N1 C1 175.1(4) . . . . ? N2 Co1 N1 C7 -118.1(5) . . . . ? O2 Co1 N1 C7 62.5(5) . . . . ? N3 Co1 N1 C7 -27.9(5) . . . . ? N4 Co1 N1 C7 153.6(5) . . . . ? Mo1 Co1 N1 C7 56.4(6) . . . . ? C3 C2 N2 C6 2.8(11) . . . . ? C1 C2 N2 C6 -176.9(7) . . . . ? C3 C2 N2 Co1 -175.6(6) . . . . ? C1 C2 N2 Co1 4.7(8) . . . . ? C5 C6 N2 C2 -3.0(11) . . . . ? C5 C6 N2 Co1 175.3(6) . . . . ? O1 Co1 N2 C2 176.2(5) . . . . ? N3 Co1 N2 C2 -88.7(5) . . . . ? N4 Co1 N2 C2 80.9(5) . . . . ? N1 Co1 N2 C2 -3.1(5) . . . . ? Mo1 Co1 N2 C2 -178.6(4) . . . . ? O1 Co1 N2 C6 -2.1(6) . . . . ? N3 Co1 N2 C6 93.0(6) . . . . ? N4 Co1 N2 C6 -97.4(6) . . . . ? N1 Co1 N2 C6 178.6(6) . . . . ? Mo1 Co1 N2 C6 3.1(7) . . . . ? C11 C12 N3 C8 2.9(11) . . . . ? C11 C12 N3 Co1 174.8(6) . . . . ? C9 C8 N3 C12 -1.7(10) . . . . ? C7 C8 N3 C12 -179.6(7) . . . . ? C9 C8 N3 Co1 -174.6(5) . . . . ? C7 C8 N3 Co1 7.5(8) . . . . ? O1 Co1 N3 C12 22.4(6) . . . . ? N2 Co1 N3 C12 -72.8(6) . . . . ? O2 Co1 N3 C12 102.0(6) . . . . ? N4 Co1 N3 C12 -151.9(12) . . . . ? N1 Co1 N3 C12 -159.7(6) . . . . ? Mo1 Co1 N3 C12 58.1(6) . . . . ? O1 Co1 N3 C8 -165.1(5) . . . . ? N2 Co1 N3 C8 99.7(5) . . . . ? O2 Co1 N3 C8 -85.4(5) . . . . ? N4 Co1 N3 C8 20.6(17) . . . . ? N1 Co1 N3 C8 12.8(5) . . . . ? Mo1 Co1 N3 C8 -129.4(5) . . . . ? C15 C14 N4 C18 1.8(11) . . . . ? C13 C14 N4 C18 -175.7(6) . . . . ? C15 C14 N4 Co1 175.7(6) . . . . ? C13 C14 N4 Co1 -1.8(8) . . . . ? C17 C18 N4 C14 0.7(10) . . . . ? C17 C18 N4 Co1 -172.5(5) . . . . ? O1 Co1 N4 C14 160.5(5) . . . . ? N2 Co1 N4 C14 -104.5(5) . . . . ? O2 Co1 N4 C14 80.7(5) . . . . ? N3 Co1 N4 C14 -25.3(17) . . . . ? N1 Co1 N4 C14 -17.4(5) . . . . ? Mo1 Co1 N4 C14 124.3(5) . . . . ? O1 Co1 N4 C18 -25.9(6) . . . . ? N2 Co1 N4 C18 69.1(6) . . . . ? O2 Co1 N4 C18 -105.7(6) . . . . ? N3 Co1 N4 C18 148.3(12) . . . . ? N1 Co1 N4 C18 156.2(6) . . . . ? Mo1 Co1 N4 C18 -62.1(6) . . . . ? O4 Mo1 O1 Co1 -100.5(3) . . . . ? O3 Mo1 O1 Co1 148.0(3) . . . . ? O2 Mo1 O1 Co1 38.5(4) 7_566 . . . ? O2 Mo1 O1 Co1 6.8(2) . . . . ? N2 Co1 O1 Mo1 173.3(3) . . . . ? O2 Co1 O1 Mo1 -7.3(2) . . . . ? N3 Co1 O1 Mo1 82.8(3) . . . . ? N4 Co1 O1 Mo1 -98.3(3) . . . . ? O1 Co1 O2 Mo1 -145.7(6) . . . 7_566 ? N3 Co1 O2 Mo1 119.3(6) . . . 7_566 ? N4 Co1 O2 Mo1 -50.6(6) . . . 7_566 ? N1 Co1 O2 Mo1 33.6(6) . . . 7_566 ? Mo1 Co1 O2 Mo1 -151.9(7) . . . 7_566 ? O1 Co1 O2 Mo1 6.2(2) . . . . ? N3 Co1 O2 Mo1 -88.8(3) . . . . ? N4 Co1 O2 Mo1 101.3(2) . . . . ? N1 Co1 O2 Mo1 -174.5(2) . . . . ? O4 Mo1 O2 Co1 96.1(2) . . . . ? O3 Mo1 O2 Co1 -95.2(4) . . . . ? O1 Mo1 O2 Co1 -6.4(2) . . . . ? O2 Mo1 O2 Co1 -166.1(4) 7_566 . . . ? O4 Mo1 O2 Mo1 -97.8(3) . . . 7_566 ? O3 Mo1 O2 Mo1 70.9(4) . . . 7_566 ? O1 Mo1 O2 Mo1 159.8(3) . . . 7_566 ? O2 Mo1 O2 Mo1 0.0 7_566 . . 7_566 ? Co1 Mo1 O2 Mo1 166.1(4) . . . 7_566 ? F102 C100 S100 O101 -57.8(7) . . . . ? F103 C100 S100 O101 63.0(7) . . . . ? F101 C100 S100 O101 -177.3(6) . . . . ? F102 C100 S100 O102 -177.0(6) . . . . ? F103 C100 S100 O102 -56.2(7) . . . . ? F101 C100 S100 O102 63.5(7) . . . . ? F102 C100 S100 O103 63.1(7) . . . . ? F103 C100 S100 O103 -176.2(6) . . . . ? F101 C100 S100 O103 -56.4(7) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 936998' ####################################################################### # # 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_c:jf180-3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H36 Fe2 Mo2 N8 O8, 2(C2 H3 N)' _chemical_formula_sum 'C40 H42 Fe2 Mo2 N10 O8' _chemical_formula_weight 1094.42 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' Fe Fe 0.3463 0.8444 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2347(4) _cell_length_b 10.7794(6) _cell_length_c 11.9562(6) _cell_angle_alpha 88.958(4) _cell_angle_beta 86.074(4) _cell_angle_gamma 89.140(5) _cell_volume 1058.53(9) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 32925 _cell_measurement_theta_min 3.42 _cell_measurement_theta_max 29.57 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 552 _exptl_absorpt_coefficient_mu 1.315 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'STOE X-RED' _exptl_absorpt_correction_T_min 0.7800 _exptl_absorpt_correction_T_max 0.9314 loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 -5 -1 0.0070 0 5 1 0.0460 -5 0 -1 0.1600 6 0 1 0.1310 0 1 -5 0.0290 0 -1 5 0.0650 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 2T' _diffrn_detector 'image plate (34 cm diameter)' _diffrn_detector_type STOE _diffrn_detector_area_resol_mean 6.67 _diffrn_source 'sealed X-ray tube, 12 x 0.4 mm long-fine focus' _diffrn_source_voltage 50 _diffrn_source_current 45 _diffrn_source_power 2.25 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_polarisn_norm 0 _diffrn_radiation_collimation '0.5 mm diameter, monocapillary' _diffrn_measurement_method 'rotation method' _diffrn_measurement_details ; 515 frames, detector distance = 100 mm ; _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_number 21217 _diffrn_reflns_theta_min 3.42 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_full 26.00 _diffrn_reflns_av_unetI/netI 0.0582 _diffrn_reflns_av_R_equivalents 0.0899 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _reflns_d_resolution_high 0.811 _reflns_d_resolution_low 5.963 _reflns_special_details 'Friedel pairs have been merged' _reflns_limit_h_min -10 _reflns_limit_h_max 10 _reflns_limit_k_min -13 _reflns_limit_k_max 13 _reflns_limit_l_min 0 _reflns_limit_l_max 14 _reflns_number_total 4154 _reflns_number_gt 3162 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _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^)+(0.0605P)^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 4154 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0477 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0895 _refine_ls_wR_factor_gt 0.0880 _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_restrained_S_all 0.904 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.754 _refine_diff_density_min -1.656 _refine_diff_density_rms 0.122 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 C1 C 0.4284(4) -0.4038(4) 0.6543(3) 0.0218(8) Uani 1 1 d . . . H11 H 0.4230 -0.4938 0.6721 0.026 Uiso 1 1 calc R . . H12 H 0.3946 -0.3905 0.5771 0.026 Uiso 1 1 calc R . . C2 C 0.3139(4) -0.3347(4) 0.7347(3) 0.0208(8) Uani 1 1 d . . . C3 C 0.1846(5) -0.3930(4) 0.7946(3) 0.0250(8) Uani 1 1 d . . . H31 H 0.1694 -0.4798 0.7890 0.030 Uiso 1 1 calc R . . C4 C 0.0793(5) -0.3220(4) 0.8620(3) 0.0283(9) Uani 1 1 d . . . H41 H -0.0088 -0.3595 0.9048 0.034 Uiso 1 1 calc R . . C5 C 0.1030(5) -0.1959(4) 0.8669(3) 0.0275(9) Uani 1 1 d . . . H51 H 0.0301 -0.1451 0.9116 0.033 Uiso 1 1 calc R . . C6 C 0.2349(5) -0.1446(4) 0.8057(3) 0.0218(8) Uani 1 1 d . . . H61 H 0.2516 -0.0578 0.8097 0.026 Uiso 1 1 calc R . . C7 C 0.6977(5) -0.3900(4) 0.5568(3) 0.0207(8) Uani 1 1 d . . . H71 H 0.6314 -0.3780 0.4914 0.025 Uiso 1 1 calc R . . H72 H 0.7344 -0.4779 0.5591 0.025 Uiso 1 1 calc R . . C8 C 0.8442(5) -0.3068(3) 0.5440(3) 0.0197(8) Uani 1 1 d . . . C9 C 0.9810(5) -0.3377(4) 0.4754(3) 0.0248(8) Uani 1 1 d . . . H91 H 0.9844 -0.4119 0.4337 0.030 Uiso 1 1 calc R . . C10 C 1.1119(5) -0.2591(4) 0.4687(3) 0.0249(8) Uani 1 1 d . . . H101 H 1.2067 -0.2786 0.4222 0.030 Uiso 1 1 calc R . . C11 C 1.1042(5) -0.1521(4) 0.5298(3) 0.0252(8) Uani 1 1 d . . . H111 H 1.1943 -0.0979 0.5285 0.030 Uiso 1 1 calc R . . C12 C 0.9609(5) -0.1254(4) 0.5937(3) 0.0225(8) Uani 1 1 d . . . H121 H 0.9540 -0.0505 0.6346 0.027 Uiso 1 1 calc R . . C13 C 0.6743(5) -0.4156(4) 0.7595(3) 0.0215(8) Uani 1 1 d . . . H131 H 0.7920 -0.4287 0.7401 0.026 Uiso 1 1 calc R . . H132 H 0.6261 -0.4976 0.7781 0.026 Uiso 1 1 calc R . . C14 C 0.6528(4) -0.3342(4) 0.8613(3) 0.0191(7) Uani 1 1 d . . . C15 C 0.6536(5) -0.3845(4) 0.9694(3) 0.0242(8) Uani 1 1 d . . . H151 H 0.6611 -0.4717 0.9812 0.029 Uiso 1 1 calc R . . C16 C 0.6433(5) -0.3053(4) 1.0593(3) 0.0278(9) Uani 1 1 d . . . H161 H 0.6433 -0.3373 1.1339 0.033 Uiso 1 1 calc R . . C17 C 0.6328(5) -0.1779(4) 1.0390(3) 0.0271(9) Uani 1 1 d . . . H171 H 0.6255 -0.1215 1.0994 0.033 Uiso 1 1 calc R . . C18 C 0.6333(5) -0.1354(4) 0.9302(3) 0.0231(8) Uani 1 1 d . . . H181 H 0.6260 -0.0485 0.9166 0.028 Uiso 1 1 calc R . . C19 C 0.9139(5) 0.2804(4) 0.8369(3) 0.0259(9) Uani 1 1 d . . . C20 C 0.9051(5) 0.1490(4) 0.8124(4) 0.0304(9) Uani 1 1 d . . . H20A H 1.0034 0.1234 0.7673 0.046 Uiso 1 1 calc R . . H20B H 0.8091 0.1344 0.7707 0.046 Uiso 1 1 calc R . . H20C H 0.8970 0.1008 0.8828 0.046 Uiso 1 1 calc R . . Fe1 Fe 0.58644(6) -0.15382(5) 0.67319(4) 0.01716(14) Uani 1 1 d . . . Mo1 Mo 0.46119(4) 0.14581(3) 0.63700(3) 0.01807(10) Uani 1 1 d . . . N1 N 0.5977(4) -0.3617(3) 0.6605(3) 0.0195(7) Uani 1 1 d . . . N2 N 0.3402(4) -0.2126(3) 0.7408(3) 0.0195(6) Uani 1 1 d . . . N3 N 0.8322(4) -0.2002(3) 0.6003(3) 0.0199(7) Uani 1 1 d . . . N4 N 0.6438(4) -0.2114(3) 0.8418(3) 0.0194(6) Uani 1 1 d . . . N5 N 0.9231(5) 0.3828(4) 0.8561(3) 0.0361(9) Uani 1 1 d . . . O1 O 0.5841(3) 0.0251(2) 0.7001(2) 0.0213(6) Uani 1 1 d . . . O2 O 0.2580(3) 0.1231(3) 0.6781(3) 0.0337(7) Uani 1 1 d . . . O3 O 0.4909(3) 0.1478(2) 0.4893(2) 0.0209(6) Uani 1 1 d . . . O4 O 0.5190(4) 0.2894(3) 0.6833(2) 0.0285(6) 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 C1 0.0155(18) 0.0214(19) 0.029(2) -0.0027(15) -0.0060(15) -0.0030(15) C2 0.0126(17) 0.025(2) 0.0258(19) -0.0018(15) -0.0072(15) -0.0024(15) C3 0.0186(19) 0.024(2) 0.033(2) 0.0023(17) -0.0066(16) -0.0078(16) C4 0.0166(19) 0.039(2) 0.030(2) 0.0036(18) -0.0030(16) -0.0065(17) C5 0.0146(19) 0.040(3) 0.028(2) -0.0034(18) -0.0010(16) 0.0019(17) C6 0.0152(18) 0.025(2) 0.026(2) -0.0010(16) -0.0016(15) -0.0020(15) C7 0.0189(19) 0.0203(19) 0.0231(19) -0.0053(15) -0.0019(15) 0.0002(15) C8 0.0180(18) 0.0190(18) 0.0226(19) -0.0002(15) -0.0048(15) 0.0020(15) C9 0.025(2) 0.023(2) 0.026(2) -0.0027(16) -0.0012(16) 0.0043(16) C10 0.0174(19) 0.028(2) 0.029(2) 0.0020(17) 0.0007(16) 0.0037(16) C11 0.0172(19) 0.028(2) 0.030(2) 0.0034(17) 0.0023(16) -0.0010(16) C12 0.0200(19) 0.025(2) 0.0228(19) -0.0005(15) -0.0041(15) -0.0015(16) C13 0.0198(19) 0.0202(19) 0.025(2) -0.0012(15) -0.0032(15) -0.0005(15) C14 0.0103(16) 0.0235(19) 0.0238(19) -0.0030(15) -0.0034(14) -0.0007(14) C15 0.0193(19) 0.023(2) 0.030(2) 0.0017(16) -0.0002(16) 0.0019(15) C16 0.026(2) 0.036(2) 0.0212(19) 0.0001(17) -0.0006(16) 0.0012(18) C17 0.031(2) 0.028(2) 0.022(2) -0.0069(16) 0.0000(17) -0.0005(17) C18 0.022(2) 0.0219(19) 0.026(2) -0.0049(16) -0.0026(16) -0.0004(16) C19 0.019(2) 0.031(2) 0.027(2) 0.0006(17) -0.0044(16) -0.0012(17) C20 0.027(2) 0.032(2) 0.033(2) -0.0017(18) -0.0014(18) -0.0024(18) Fe1 0.0142(3) 0.0172(3) 0.0203(3) -0.0032(2) -0.0019(2) -0.0001(2) Mo1 0.01451(16) 0.01950(18) 0.02013(17) -0.00186(12) -0.00041(12) 0.00077(12) N1 0.0154(16) 0.0198(16) 0.0237(16) -0.0035(13) -0.0046(13) -0.0001(12) N2 0.0130(15) 0.0234(16) 0.0223(16) -0.0016(13) -0.0027(12) -0.0025(12) N3 0.0172(16) 0.0203(16) 0.0224(16) -0.0013(13) -0.0028(12) 0.0025(13) N4 0.0136(15) 0.0213(16) 0.0236(16) -0.0030(13) -0.0018(12) -0.0002(12) N5 0.031(2) 0.033(2) 0.045(2) 0.0002(17) -0.0064(17) -0.0034(17) O1 0.0180(13) 0.0217(14) 0.0250(14) -0.0036(11) -0.0056(11) -0.0016(11) O2 0.0176(14) 0.0429(18) 0.0393(17) 0.0110(14) 0.0036(12) 0.0023(13) O3 0.0180(13) 0.0203(13) 0.0251(14) -0.0029(11) -0.0050(11) 0.0011(11) O4 0.0385(17) 0.0235(14) 0.0235(14) -0.0029(11) -0.0026(12) 0.0033(13) _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 C1 N1 1.480(5) . ? C1 C2 1.500(5) . ? C1 H11 0.9900 . ? C1 H12 0.9900 . ? C2 N2 1.341(5) . ? C2 C3 1.393(6) . ? C3 C4 1.376(6) . ? C3 H31 0.9500 . ? C4 C5 1.380(6) . ? C4 H41 0.9500 . ? C5 C6 1.384(6) . ? C5 H51 0.9500 . ? C6 N2 1.342(5) . ? C6 H61 0.9500 . ? C7 N1 1.475(5) . ? C7 C8 1.512(5) . ? C7 H71 0.9900 . ? C7 H72 0.9900 . ? C8 N3 1.341(5) . ? C8 C9 1.387(5) . ? C9 C10 1.379(6) . ? C9 H91 0.9500 . ? C10 C11 1.375(6) . ? C10 H101 0.9500 . ? C11 C12 1.390(6) . ? C11 H111 0.9500 . ? C12 N3 1.339(5) . ? C12 H121 0.9500 . ? C13 N1 1.484(5) . ? C13 C14 1.512(5) . ? C13 H131 0.9900 . ? C13 H132 0.9900 . ? C14 N4 1.341(5) . ? C14 C15 1.393(5) . ? C15 C16 1.382(6) . ? C15 H151 0.9500 . ? C16 C17 1.392(6) . ? C16 H161 0.9500 . ? C17 C18 1.371(6) . ? C17 H171 0.9500 . ? C18 N4 1.346(5) . ? C18 H181 0.9500 . ? C19 N5 1.137(6) . ? C19 C20 1.455(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? Fe1 O1 1.961(3) . ? Fe1 O3 2.085(3) 2_656 ? Fe1 N4 2.180(3) . ? Fe1 N3 2.202(3) . ? Fe1 N2 2.228(3) . ? Fe1 N1 2.249(3) . ? Mo1 O2 1.731(3) . ? Mo1 O4 1.737(3) . ? Mo1 O3 1.766(3) . ? Mo1 O1 1.821(3) . ? O3 Fe1 2.085(3) 2_656 ? 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 N1 C1 C2 111.1(3) . . ? N1 C1 H11 109.4 . . ? C2 C1 H11 109.4 . . ? N1 C1 H12 109.4 . . ? C2 C1 H12 109.4 . . ? H11 C1 H12 108.0 . . ? N2 C2 C3 122.6(4) . . ? N2 C2 C1 115.4(3) . . ? C3 C2 C1 121.9(4) . . ? C4 C3 C2 118.5(4) . . ? C4 C3 H31 120.8 . . ? C2 C3 H31 120.8 . . ? C3 C4 C5 119.4(4) . . ? C3 C4 H41 120.3 . . ? C5 C4 H41 120.3 . . ? C4 C5 C6 118.9(4) . . ? C4 C5 H51 120.6 . . ? C6 C5 H51 120.6 . . ? N2 C6 C5 122.6(4) . . ? N2 C6 H61 118.7 . . ? C5 C6 H61 118.7 . . ? N1 C7 C8 110.6(3) . . ? N1 C7 H71 109.5 . . ? C8 C7 H71 109.5 . . ? N1 C7 H72 109.5 . . ? C8 C7 H72 109.5 . . ? H71 C7 H72 108.1 . . ? N3 C8 C9 122.1(4) . . ? N3 C8 C7 116.1(3) . . ? C9 C8 C7 121.7(3) . . ? C10 C9 C8 119.0(4) . . ? C10 C9 H91 120.5 . . ? C8 C9 H91 120.5 . . ? C11 C10 C9 119.5(4) . . ? C11 C10 H101 120.3 . . ? C9 C10 H101 120.3 . . ? C10 C11 C12 118.2(4) . . ? C10 C11 H111 120.9 . . ? C12 C11 H111 120.9 . . ? N3 C12 C11 123.1(4) . . ? N3 C12 H121 118.5 . . ? C11 C12 H121 118.5 . . ? N1 C13 C14 112.9(3) . . ? N1 C13 H131 109.0 . . ? C14 C13 H131 109.0 . . ? N1 C13 H132 109.0 . . ? C14 C13 H132 109.0 . . ? H131 C13 H132 107.8 . . ? N4 C14 C15 122.0(3) . . ? N4 C14 C13 116.6(3) . . ? C15 C14 C13 121.2(3) . . ? C16 C15 C14 118.9(4) . . ? C16 C15 H151 120.6 . . ? C14 C15 H151 120.6 . . ? C15 C16 C17 119.0(4) . . ? C15 C16 H161 120.5 . . ? C17 C16 H161 120.5 . . ? C18 C17 C16 118.7(4) . . ? C18 C17 H171 120.7 . . ? C16 C17 H171 120.7 . . ? N4 C18 C17 122.9(4) . . ? N4 C18 H181 118.5 . . ? C17 C18 H181 118.5 . . ? N5 C19 C20 179.0(4) . . ? 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 . . ? O1 Fe1 O3 98.23(11) . 2_656 ? O1 Fe1 N4 96.28(11) . . ? O3 Fe1 N4 164.48(11) 2_656 . ? O1 Fe1 N3 106.32(11) . . ? O3 Fe1 N3 87.96(11) 2_656 . ? N4 Fe1 N3 93.22(11) . . ? O1 Fe1 N2 103.27(11) . . ? O3 Fe1 N2 90.72(11) 2_656 . ? N4 Fe1 N2 80.61(11) . . ? N3 Fe1 N2 150.27(12) . . ? O1 Fe1 N1 174.02(11) . . ? O3 Fe1 N1 87.75(11) 2_656 . ? N4 Fe1 N1 77.76(12) . . ? N3 Fe1 N1 73.79(12) . . ? N2 Fe1 N1 76.47(12) . . ? O2 Mo1 O4 109.01(15) . . ? O2 Mo1 O3 110.39(14) . . ? O4 Mo1 O3 107.47(13) . . ? O2 Mo1 O1 109.31(13) . . ? O4 Mo1 O1 108.98(13) . . ? O3 Mo1 O1 111.62(12) . . ? C7 N1 C1 111.3(3) . . ? C7 N1 C13 110.3(3) . . ? C1 N1 C13 111.9(3) . . ? C7 N1 Fe1 106.8(2) . . ? C1 N1 Fe1 106.8(2) . . ? C13 N1 Fe1 109.5(2) . . ? C2 N2 C6 118.0(3) . . ? C2 N2 Fe1 114.4(2) . . ? C6 N2 Fe1 125.9(3) . . ? C12 N3 C8 118.0(3) . . ? C12 N3 Fe1 126.2(3) . . ? C8 N3 Fe1 115.0(2) . . ? C14 N4 C18 118.5(3) . . ? C14 N4 Fe1 116.0(2) . . ? C18 N4 Fe1 123.7(3) . . ? Mo1 O1 Fe1 128.36(14) . . ? Mo1 O3 Fe1 154.31(15) . 2_656 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 41.6(4) . . . . ? N1 C1 C2 C3 -141.5(4) . . . . ? N2 C2 C3 C4 0.4(6) . . . . ? C1 C2 C3 C4 -176.4(4) . . . . ? C2 C3 C4 C5 1.1(6) . . . . ? C3 C4 C5 C6 -1.5(6) . . . . ? C4 C5 C6 N2 0.6(6) . . . . ? N1 C7 C8 N3 -22.0(4) . . . . ? N1 C7 C8 C9 159.8(3) . . . . ? N3 C8 C9 C10 3.0(6) . . . . ? C7 C8 C9 C10 -178.9(3) . . . . ? C8 C9 C10 C11 0.0(6) . . . . ? C9 C10 C11 C12 -2.1(6) . . . . ? C10 C11 C12 N3 1.6(6) . . . . ? N1 C13 C14 N4 -30.7(5) . . . . ? N1 C13 C14 C15 153.5(3) . . . . ? N4 C14 C15 C16 0.6(6) . . . . ? C13 C14 C15 C16 176.1(4) . . . . ? C14 C15 C16 C17 -0.2(6) . . . . ? C15 C16 C17 C18 -0.1(6) . . . . ? C16 C17 C18 N4 -0.1(6) . . . . ? C8 C7 N1 C1 158.1(3) . . . . ? C8 C7 N1 C13 -77.0(4) . . . . ? C8 C7 N1 Fe1 41.9(3) . . . . ? C2 C1 N1 C7 -157.9(3) . . . . ? C2 C1 N1 C13 78.1(4) . . . . ? C2 C1 N1 Fe1 -41.7(3) . . . . ? C14 C13 N1 C7 143.7(3) . . . . ? C14 C13 N1 C1 -91.8(4) . . . . ? C14 C13 N1 Fe1 26.5(4) . . . . ? O3 Fe1 N1 C7 52.6(2) 2_656 . . . ? N4 Fe1 N1 C7 -133.0(2) . . . . ? N3 Fe1 N1 C7 -35.9(2) . . . . ? N2 Fe1 N1 C7 143.9(2) . . . . ? O3 Fe1 N1 C1 -66.6(2) 2_656 . . . ? N4 Fe1 N1 C1 107.8(2) . . . . ? N3 Fe1 N1 C1 -155.1(3) . . . . ? N2 Fe1 N1 C1 24.7(2) . . . . ? O3 Fe1 N1 C13 172.0(2) 2_656 . . . ? N4 Fe1 N1 C13 -13.5(2) . . . . ? N3 Fe1 N1 C13 83.5(2) . . . . ? N2 Fe1 N1 C13 -96.7(2) . . . . ? C3 C2 N2 C6 -1.3(5) . . . . ? C1 C2 N2 C6 175.6(3) . . . . ? C3 C2 N2 Fe1 164.9(3) . . . . ? C1 C2 N2 Fe1 -18.1(4) . . . . ? C5 C6 N2 C2 0.8(6) . . . . ? C5 C6 N2 Fe1 -163.7(3) . . . . ? O1 Fe1 N2 C2 -178.1(2) . . . . ? O3 Fe1 N2 C2 83.3(3) 2_656 . . . ? N4 Fe1 N2 C2 -83.8(3) . . . . ? N3 Fe1 N2 C2 -3.8(4) . . . . ? N1 Fe1 N2 C2 -4.2(2) . . . . ? O1 Fe1 N2 C6 -13.1(3) . . . . ? O3 Fe1 N2 C6 -111.7(3) 2_656 . . . ? N4 Fe1 N2 C6 81.2(3) . . . . ? N3 Fe1 N2 C6 161.2(3) . . . . ? N1 Fe1 N2 C6 160.8(3) . . . . ? C11 C12 N3 C8 1.2(6) . . . . ? C11 C12 N3 Fe1 -168.5(3) . . . . ? C9 C8 N3 C12 -3.6(5) . . . . ? C7 C8 N3 C12 178.2(3) . . . . ? C9 C8 N3 Fe1 167.3(3) . . . . ? C7 C8 N3 Fe1 -10.9(4) . . . . ? O1 Fe1 N3 C12 10.2(3) . . . . ? O3 Fe1 N3 C12 108.1(3) 2_656 . . . ? N4 Fe1 N3 C12 -87.4(3) . . . . ? N2 Fe1 N3 C12 -164.0(3) . . . . ? N1 Fe1 N3 C12 -163.6(3) . . . . ? O1 Fe1 N3 C8 -159.8(2) . . . . ? O3 Fe1 N3 C8 -61.9(3) 2_656 . . . ? N4 Fe1 N3 C8 102.7(3) . . . . ? N2 Fe1 N3 C8 26.0(4) . . . . ? N1 Fe1 N3 C8 26.4(3) . . . . ? C15 C14 N4 C18 -0.8(5) . . . . ? C13 C14 N4 C18 -176.5(3) . . . . ? C15 C14 N4 Fe1 -166.0(3) . . . . ? C13 C14 N4 Fe1 18.3(4) . . . . ? C17 C18 N4 C14 0.6(6) . . . . ? C17 C18 N4 Fe1 164.5(3) . . . . ? O1 Fe1 N4 C14 178.2(3) . . . . ? O3 Fe1 N4 C14 19.0(6) 2_656 . . . ? N3 Fe1 N4 C14 -75.0(3) . . . . ? N2 Fe1 N4 C14 75.7(3) . . . . ? N1 Fe1 N4 C14 -2.3(3) . . . . ? O1 Fe1 N4 C18 13.9(3) . . . . ? O3 Fe1 N4 C18 -145.3(4) 2_656 . . . ? N3 Fe1 N4 C18 120.7(3) . . . . ? N2 Fe1 N4 C18 -88.6(3) . . . . ? N1 Fe1 N4 C18 -166.6(3) . . . . ? O2 Mo1 O1 Fe1 65.3(2) . . . . ? O4 Mo1 O1 Fe1 -175.62(17) . . . . ? O3 Mo1 O1 Fe1 -57.1(2) . . . . ? O3 Fe1 O1 Mo1 26.4(2) 2_656 . . . ? N4 Fe1 O1 Mo1 -148.14(18) . . . . ? N3 Fe1 O1 Mo1 116.63(18) . . . . ? N2 Fe1 O1 Mo1 -66.3(2) . . . . ? O2 Mo1 O3 Fe1 11.2(4) . . . 2_656 ? O4 Mo1 O3 Fe1 -107.6(3) . . . 2_656 ? O1 Mo1 O3 Fe1 132.9(3) . . . 2_656 ? _database_code_depnum_ccdc_archive 'CCDC 936999' ####################################################################### # # 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_jf250 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H36 Fe2 Mo N8 O5, 2(C F3 O3 S)' _chemical_formula_sum 'C38 H36 F6 Fe2 Mo N8 O11 S2' _chemical_formula_weight 1166.51 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.0539(4) _cell_length_b 14.1854(5) _cell_length_c 16.1221(7) _cell_angle_alpha 84.611(3) _cell_angle_beta 78.110(3) _cell_angle_gamma 78.873(3) _cell_volume 2204.17(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 34914 _cell_measurement_theta_min 3.27 _cell_measurement_theta_max 29.59 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.758 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 1.118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6824 _exptl_absorpt_correction_T_max 0.8156 _exptl_absorpt_process_details 'spek, 2003' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'STOE IPDS2theta' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 'no decay' _diffrn_reflns_number 33490 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0388 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 29.57 _reflns_number_total 12261 _reflns_number_gt 9651 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_cell_refinement 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-RED (Stoe & Cie, 2002)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON, 1990' _computing_publication_material 'PLATON, 1990' _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^)+(0.0481P)^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 12261 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0773 _refine_ls_wR_factor_gt 0.0722 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _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 C1 C 0.1182(2) 0.13985(14) 0.89739(12) 0.0200(4) Uani 1 1 d . . . H1A H 0.0719 0.0966 0.9409 0.024 Uiso 1 1 calc R . . H1B H 0.0696 0.2067 0.9069 0.024 Uiso 1 1 calc R . . C2 C 0.2669(2) 0.13071(13) 0.90541(12) 0.0188(4) Uani 1 1 d . . . C3 C 0.3092(2) 0.11536(14) 0.98281(13) 0.0227(4) Uani 1 1 d . . . H3 H 0.2447 0.1075 1.0339 0.027 Uiso 1 1 calc R . . C4 C 0.4477(2) 0.11162(15) 0.98444(14) 0.0258(4) Uani 1 1 d . . . H4 H 0.4783 0.1037 1.0371 0.031 Uiso 1 1 calc R . . C5 C 0.5413(2) 0.11958(15) 0.90874(14) 0.0253(4) Uani 1 1 d . . . H5 H 0.6368 0.1154 0.9085 0.030 Uiso 1 1 calc R . . C6 C 0.4920(2) 0.13372(14) 0.83383(13) 0.0215(4) Uani 1 1 d . . . H6 H 0.5555 0.1382 0.7817 0.026 Uiso 1 1 calc R . . C7 C 0.1389(2) 0.00787(13) 0.80611(13) 0.0201(4) Uani 1 1 d . . . H7A H 0.0503 -0.0146 0.8107 0.024 Uiso 1 1 calc R . . H7B H 0.1811 -0.0225 0.8546 0.024 Uiso 1 1 calc R . . C8 C 0.2331(2) -0.02428(13) 0.72495(13) 0.0181(4) Uani 1 1 d . . . C9 C 0.2247(2) -0.10730(14) 0.68811(14) 0.0239(4) Uani 1 1 d . . . H9 H 0.1527 -0.1425 0.7107 0.029 Uiso 1 1 calc R . . C10 C 0.3231(2) -0.13722(14) 0.61817(15) 0.0277(5) Uani 1 1 d . . . H10 H 0.3183 -0.1926 0.5908 0.033 Uiso 1 1 calc R . . C11 C 0.4286(2) -0.08601(14) 0.58810(14) 0.0258(4) Uani 1 1 d . . . H11 H 0.5006 -0.1079 0.5422 0.031 Uiso 1 1 calc R . . C12 C 0.4277(2) -0.00225(14) 0.62592(13) 0.0218(4) Uani 1 1 d . . . H12 H 0.4987 0.0341 0.6043 0.026 Uiso 1 1 calc R . . C13 C -0.0219(2) 0.15748(14) 0.78637(12) 0.0188(4) Uani 1 1 d . . . H13A H -0.0507 0.2244 0.8043 0.023 Uiso 1 1 calc R . . H13B H -0.0943 0.1203 0.8144 0.023 Uiso 1 1 calc R . . C14 C -0.0049(2) 0.15679(13) 0.69139(12) 0.0176(4) Uani 1 1 d . . . C15 C -0.1091(2) 0.14268(15) 0.65221(14) 0.0234(4) Uani 1 1 d . . . H15 H -0.1961 0.1334 0.6850 0.028 Uiso 1 1 calc R . . C16 C -0.0848(3) 0.14229(17) 0.56459(15) 0.0296(5) Uani 1 1 d . . . H16 H -0.1549 0.1326 0.5365 0.035 Uiso 1 1 calc R . . C17 C 0.0427(2) 0.15622(15) 0.51829(14) 0.0266(4) Uani 1 1 d . . . H17 H 0.0618 0.1558 0.4581 0.032 Uiso 1 1 calc R . . C18 C 0.1421(2) 0.17080(13) 0.56178(12) 0.0204(4) Uani 1 1 d . . . H18 H 0.2297 0.1805 0.5303 0.024 Uiso 1 1 calc R . . C19 C 0.1308(2) 0.61760(13) 0.62091(13) 0.0212(4) Uani 1 1 d . . . H19A H 0.1992 0.6104 0.5671 0.025 Uiso 1 1 calc R . . H19B H 0.0883 0.6865 0.6246 0.025 Uiso 1 1 calc R . . C20 C 0.0204(2) 0.55952(13) 0.62005(12) 0.0195(4) Uani 1 1 d . . . C21 C -0.0908(2) 0.59411(15) 0.58008(14) 0.0255(4) Uani 1 1 d . . . H21 H -0.1056 0.6588 0.5577 0.031 Uiso 1 1 calc R . . C22 C -0.1798(2) 0.53331(17) 0.57316(14) 0.0277(4) Uani 1 1 d . . . H22 H -0.2550 0.5556 0.5448 0.033 Uiso 1 1 calc R . . C23 C -0.1586(2) 0.43987(16) 0.60776(13) 0.0244(4) Uani 1 1 d . . . H23 H -0.2177 0.3967 0.6032 0.029 Uiso 1 1 calc R . . C24 C -0.0491(2) 0.41137(14) 0.64909(12) 0.0198(4) Uani 1 1 d . . . H24 H -0.0355 0.3480 0.6747 0.024 Uiso 1 1 calc R . . C25 C 0.1326(2) 0.63897(13) 0.77025(12) 0.0201(4) Uani 1 1 d . . . H25A H 0.0808 0.7019 0.7529 0.024 Uiso 1 1 calc R . . H25B H 0.2035 0.6516 0.8001 0.024 Uiso 1 1 calc R . . C26 C 0.0349(2) 0.58513(13) 0.83048(12) 0.0170(3) Uani 1 1 d . . . C27 C -0.0722(2) 0.63282(14) 0.88878(13) 0.0223(4) Uani 1 1 d . . . H27 H -0.0878 0.7010 0.8895 0.027 Uiso 1 1 calc R . . C28 C -0.1555(2) 0.58043(16) 0.94545(15) 0.0278(5) Uani 1 1 d . . . H28 H -0.2297 0.6118 0.9857 0.033 Uiso 1 1 calc R . . C29 C -0.1295(2) 0.48057(16) 0.94308(14) 0.0268(4) Uani 1 1 d . . . H29 H -0.1849 0.4425 0.9819 0.032 Uiso 1 1 calc R . . C30 C -0.0216(2) 0.43820(14) 0.88318(13) 0.0209(4) Uani 1 1 d . . . H30 H -0.0043 0.3701 0.8812 0.025 Uiso 1 1 calc R . . C31 C 0.3496(2) 0.59669(14) 0.67164(13) 0.0209(4) Uani 1 1 d . . . H31A H 0.3574 0.6646 0.6755 0.025 Uiso 1 1 calc R . . H31B H 0.3885 0.5787 0.6125 0.025 Uiso 1 1 calc R . . C32 C 0.4299(2) 0.53345(14) 0.73092(13) 0.0205(4) Uani 1 1 d . . . C33 C 0.5536(2) 0.55194(16) 0.74478(14) 0.0263(4) Uani 1 1 d . . . H33 H 0.5886 0.6072 0.7182 0.032 Uiso 1 1 calc R . . C34 C 0.6255(2) 0.48920(18) 0.79770(16) 0.0316(5) Uani 1 1 d . . . H34 H 0.7109 0.5005 0.8075 0.038 Uiso 1 1 calc R . . C35 C 0.5716(2) 0.40906(17) 0.83662(15) 0.0304(5) Uani 1 1 d . . . H35 H 0.6190 0.3651 0.8735 0.037 Uiso 1 1 calc R . . C36 C 0.4476(2) 0.39542(15) 0.82017(13) 0.0236(4) Uani 1 1 d . . . H36 H 0.4102 0.3411 0.8466 0.028 Uiso 1 1 calc R . . C37 C 0.3360(2) 0.16053(15) 0.23637(14) 0.0249(4) Uani 1 1 d . . . C38 C 0.6270(2) 0.29096(15) 0.08442(14) 0.0257(4) Uani 1 1 d . . . N1 N 0.11112(17) 0.11414(11) 0.81178(10) 0.0167(3) Uani 1 1 d . . . N2 N 0.35718(17) 0.14131(11) 0.83233(10) 0.0176(3) Uani 1 1 d . . . N3 N 0.32997(17) 0.02915(11) 0.69204(10) 0.0177(3) Uani 1 1 d . . . N4 N 0.11875(17) 0.17164(11) 0.64668(10) 0.0169(3) Uani 1 1 d . . . N5 N 0.20243(17) 0.58679(11) 0.69321(10) 0.0168(3) Uani 1 1 d . . . N6 N 0.03958(17) 0.46949(11) 0.65477(10) 0.0166(3) Uani 1 1 d . . . N7 N 0.06006(17) 0.48881(11) 0.82749(10) 0.0167(3) Uani 1 1 d . . . N8 N 0.37753(17) 0.45594(11) 0.76815(11) 0.0190(3) Uani 1 1 d . . . O1 O 0.19594(14) 0.30399(9) 0.75294(8) 0.0167(3) Uani 1 1 d . . . O2 O 0.42526(14) 0.20625(9) 0.63695(9) 0.0199(3) Uani 1 1 d . . . O3 O 0.33457(15) 0.41175(9) 0.60954(9) 0.0201(3) Uani 1 1 d . . . O4 O 0.62402(16) 0.32745(11) 0.55079(11) 0.0294(3) Uani 1 1 d . . . O5 O 0.42076(17) 0.29444(10) 0.46735(9) 0.0254(3) Uani 1 1 d . . . O6 O 0.08056(17) 0.17196(12) 0.30454(11) 0.0317(4) Uani 1 1 d . . . O7 O 0.24471(18) 0.03678(12) 0.34855(11) 0.0327(4) Uani 1 1 d . . . O8 O 0.18520(19) 0.04406(13) 0.20888(11) 0.0361(4) Uani 1 1 d . . . O9 O 0.74799(18) 0.12314(11) 0.03338(10) 0.0285(3) Uani 1 1 d . . . O10 O 0.79654(17) 0.26424(11) -0.05629(10) 0.0280(3) Uani 1 1 d . . . O11 O 0.88627(18) 0.22724(13) 0.07416(11) 0.0356(4) Uani 1 1 d . . . F1 F 0.45298(14) 0.10040(10) 0.20835(9) 0.0329(3) Uani 1 1 d . . . F2 F 0.30720(15) 0.22031(11) 0.17081(10) 0.0391(3) Uani 1 1 d . . . F3 F 0.35988(16) 0.21250(10) 0.29449(10) 0.0377(3) Uani 1 1 d . . . F4 F 0.59765(16) 0.25970(10) 0.16540(8) 0.0347(3) Uani 1 1 d . . . F5 F 0.51762(14) 0.29208(10) 0.04914(9) 0.0345(3) Uani 1 1 d . . . F6 F 0.64417(15) 0.38260(9) 0.08372(9) 0.0347(3) Uani 1 1 d . . . S1 S 0.19551(5) 0.09543(4) 0.27938(3) 0.02394(11) Uani 1 1 d . . . S2 S 0.78221(5) 0.21751(3) 0.02776(3) 0.02076(10) Uani 1 1 d . . . Fe1 Fe 0.26984(3) 0.181301(18) 0.722561(17) 0.01410(6) Uani 1 1 d . . . Fe2 Fe 0.20705(3) 0.427167(18) 0.719699(16) 0.01435(6) Uani 1 1 d . . . Mo1 Mo 0.455636(17) 0.310038(11) 0.564987(10) 0.01530(4) 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 C1 0.0218(10) 0.0212(9) 0.0153(9) 0.0013(7) -0.0014(7) -0.0035(7) C2 0.0238(10) 0.0136(8) 0.0190(9) 0.0010(7) -0.0052(7) -0.0030(7) C3 0.0301(11) 0.0213(9) 0.0173(9) -0.0002(7) -0.0062(8) -0.0047(8) C4 0.0338(12) 0.0238(10) 0.0239(10) -0.0009(8) -0.0143(9) -0.0056(9) C5 0.0253(11) 0.0243(10) 0.0292(11) 0.0000(8) -0.0123(9) -0.0049(8) C6 0.0200(10) 0.0206(9) 0.0246(10) 0.0012(7) -0.0070(8) -0.0035(7) C7 0.0205(10) 0.0155(8) 0.0237(10) 0.0032(7) -0.0021(7) -0.0061(7) C8 0.0185(9) 0.0134(8) 0.0218(9) 0.0036(7) -0.0057(7) -0.0020(7) C9 0.0252(11) 0.0154(8) 0.0312(11) 0.0016(7) -0.0049(8) -0.0057(8) C10 0.0364(13) 0.0148(8) 0.0308(11) -0.0019(8) -0.0053(9) -0.0031(8) C11 0.0286(11) 0.0168(9) 0.0272(11) -0.0021(8) 0.0022(8) 0.0001(8) C12 0.0209(10) 0.0178(8) 0.0239(10) 0.0020(7) -0.0015(8) -0.0015(7) C13 0.0161(9) 0.0196(8) 0.0201(9) 0.0010(7) -0.0033(7) -0.0032(7) C14 0.0190(9) 0.0122(8) 0.0216(9) 0.0005(6) -0.0049(7) -0.0023(7) C15 0.0202(10) 0.0242(9) 0.0278(11) 0.0005(8) -0.0078(8) -0.0064(8) C16 0.0318(12) 0.0327(11) 0.0300(11) -0.0012(9) -0.0142(9) -0.0114(10) C17 0.0343(12) 0.0266(10) 0.0213(10) 0.0002(8) -0.0095(9) -0.0075(9) C18 0.0248(10) 0.0182(8) 0.0181(9) 0.0007(7) -0.0045(7) -0.0040(8) C19 0.0275(11) 0.0163(8) 0.0202(9) 0.0046(7) -0.0076(8) -0.0045(8) C20 0.0223(10) 0.0174(8) 0.0170(9) 0.0010(7) -0.0031(7) -0.0010(7) C21 0.0263(11) 0.0240(10) 0.0236(10) 0.0056(8) -0.0069(8) 0.0007(8) C22 0.0221(10) 0.0352(11) 0.0256(11) 0.0012(9) -0.0096(8) -0.0002(9) C23 0.0210(10) 0.0314(10) 0.0222(10) -0.0030(8) -0.0051(8) -0.0066(8) C24 0.0223(10) 0.0193(8) 0.0187(9) -0.0018(7) -0.0059(7) -0.0037(7) C25 0.0242(10) 0.0145(8) 0.0208(9) -0.0011(7) -0.0012(7) -0.0050(7) C26 0.0184(9) 0.0172(8) 0.0170(9) -0.0007(7) -0.0060(7) -0.0044(7) C27 0.0219(10) 0.0198(9) 0.0259(10) -0.0060(7) -0.0047(8) -0.0029(8) C28 0.0235(11) 0.0302(11) 0.0280(11) -0.0087(9) 0.0025(8) -0.0056(9) C29 0.0267(11) 0.0284(10) 0.0249(11) -0.0009(8) 0.0006(8) -0.0102(9) C30 0.0238(10) 0.0198(9) 0.0204(9) 0.0006(7) -0.0044(7) -0.0078(8) C31 0.0202(10) 0.0181(8) 0.0247(10) 0.0006(7) -0.0022(8) -0.0074(7) C32 0.0200(10) 0.0212(9) 0.0202(9) -0.0053(7) -0.0014(7) -0.0042(7) C33 0.0215(10) 0.0291(10) 0.0296(11) -0.0084(9) -0.0013(8) -0.0080(8) C34 0.0219(11) 0.0428(13) 0.0332(12) -0.0112(10) -0.0087(9) -0.0053(10) C35 0.0280(12) 0.0366(12) 0.0272(11) -0.0043(9) -0.0117(9) 0.0011(9) C36 0.0259(11) 0.0232(9) 0.0215(10) -0.0013(7) -0.0071(8) -0.0014(8) C37 0.0260(11) 0.0241(9) 0.0251(10) 0.0027(8) -0.0073(8) -0.0051(8) C38 0.0271(11) 0.0274(10) 0.0226(10) -0.0029(8) 0.0011(8) -0.0103(9) N1 0.0162(8) 0.0160(7) 0.0175(8) 0.0002(6) -0.0022(6) -0.0033(6) N2 0.0183(8) 0.0157(7) 0.0190(8) 0.0014(6) -0.0051(6) -0.0029(6) N3 0.0175(8) 0.0142(7) 0.0206(8) 0.0012(6) -0.0043(6) -0.0013(6) N4 0.0185(8) 0.0129(7) 0.0194(8) 0.0005(6) -0.0055(6) -0.0013(6) N5 0.0189(8) 0.0160(7) 0.0153(7) 0.0015(6) -0.0024(6) -0.0049(6) N6 0.0200(8) 0.0155(7) 0.0145(7) -0.0001(6) -0.0054(6) -0.0019(6) N7 0.0182(8) 0.0171(7) 0.0153(7) 0.0001(6) -0.0043(6) -0.0040(6) N8 0.0195(8) 0.0187(7) 0.0194(8) -0.0016(6) -0.0050(6) -0.0031(6) O1 0.0183(7) 0.0148(6) 0.0166(6) 0.0008(5) -0.0030(5) -0.0032(5) O2 0.0178(7) 0.0161(6) 0.0230(7) 0.0017(5) 0.0015(5) -0.0032(5) O3 0.0257(7) 0.0158(6) 0.0165(7) 0.0011(5) 0.0004(5) -0.0038(5) O4 0.0227(8) 0.0304(8) 0.0356(9) 0.0067(6) -0.0057(6) -0.0102(6) O5 0.0319(8) 0.0216(7) 0.0225(7) -0.0029(6) -0.0062(6) -0.0021(6) O6 0.0233(8) 0.0347(8) 0.0343(9) -0.0005(7) -0.0032(7) -0.0014(7) O7 0.0340(9) 0.0309(8) 0.0342(9) 0.0088(7) -0.0082(7) -0.0113(7) O8 0.0360(10) 0.0417(9) 0.0358(9) -0.0104(7) -0.0087(7) -0.0141(8) O9 0.0382(9) 0.0212(7) 0.0301(8) 0.0003(6) -0.0151(7) -0.0070(6) O10 0.0292(8) 0.0266(7) 0.0232(8) 0.0009(6) 0.0020(6) -0.0015(6) O11 0.0288(9) 0.0468(10) 0.0369(9) -0.0137(8) -0.0117(7) -0.0092(8) F1 0.0220(7) 0.0357(7) 0.0385(8) 0.0016(6) -0.0028(6) -0.0036(5) F2 0.0331(8) 0.0431(8) 0.0376(8) 0.0177(6) -0.0088(6) -0.0061(6) F3 0.0418(8) 0.0352(7) 0.0420(8) -0.0070(6) -0.0085(7) -0.0187(6) F4 0.0415(8) 0.0400(7) 0.0220(7) -0.0019(5) 0.0047(6) -0.0173(6) F5 0.0236(7) 0.0408(8) 0.0380(8) -0.0054(6) -0.0042(6) -0.0031(6) F6 0.0406(8) 0.0240(6) 0.0352(8) -0.0073(5) 0.0090(6) -0.0100(6) S1 0.0218(2) 0.0251(2) 0.0260(3) -0.00069(19) -0.00475(19) -0.0071(2) S2 0.0219(2) 0.0220(2) 0.0200(2) -0.00251(17) -0.00607(18) -0.00483(18) Fe1 0.01501(13) 0.01197(11) 0.01523(13) 0.00169(9) -0.00289(9) -0.00336(9) Fe2 0.01677(13) 0.01176(11) 0.01469(13) 0.00053(9) -0.00381(10) -0.00277(10) Mo1 0.01506(8) 0.01389(7) 0.01656(8) 0.00085(5) -0.00143(6) -0.00414(6) _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 C1 N1 1.479(2) . ? C1 C2 1.507(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.347(3) . ? C2 C3 1.385(3) . ? C3 C4 1.389(3) . ? C3 H3 0.9500 . ? C4 C5 1.389(3) . ? C4 H4 0.9500 . ? C5 C6 1.381(3) . ? C5 H5 0.9500 . ? C6 N2 1.344(3) . ? C6 H6 0.9500 . ? C7 N1 1.487(2) . ? C7 C8 1.500(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N3 1.342(2) . ? C8 C9 1.392(3) . ? C9 C10 1.378(3) . ? C9 H9 0.9500 . ? C10 C11 1.381(3) . ? C10 H10 0.9500 . ? C11 C12 1.383(3) . ? C11 H11 0.9500 . ? C12 N3 1.337(3) . ? C12 H12 0.9500 . ? C13 N1 1.482(3) . ? C13 C14 1.506(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N4 1.346(3) . ? C14 C15 1.384(3) . ? C15 C16 1.383(3) . ? C15 H15 0.9500 . ? C16 C17 1.384(3) . ? C16 H16 0.9500 . ? C17 C18 1.389(3) . ? C17 H17 0.9500 . ? C18 N4 1.341(2) . ? C18 H18 0.9500 . ? C19 N5 1.482(3) . ? C19 C20 1.508(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 N6 1.341(2) . ? C20 C21 1.390(3) . ? C21 C22 1.383(3) . ? C21 H21 0.9500 . ? C22 C23 1.384(3) . ? C22 H22 0.9500 . ? C23 C24 1.378(3) . ? C23 H23 0.9500 . ? C24 N6 1.347(2) . ? C24 H24 0.9500 . ? C25 N5 1.482(2) . ? C25 C26 1.499(3) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 N7 1.344(2) . ? C26 C27 1.386(3) . ? C27 C28 1.373(3) . ? C27 H27 0.9500 . ? C28 C29 1.393(3) . ? C28 H28 0.9500 . ? C29 C30 1.377(3) . ? C29 H29 0.9500 . ? C30 N7 1.341(2) . ? C30 H30 0.9500 . ? C31 N5 1.479(2) . ? C31 C32 1.499(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N8 1.347(3) . ? C32 C33 1.384(3) . ? C33 C34 1.380(3) . ? C33 H33 0.9500 . ? C34 C35 1.394(4) . ? C34 H34 0.9500 . ? C35 C36 1.378(3) . ? C35 H35 0.9500 . ? C36 N8 1.346(3) . ? C36 H36 0.9500 . ? C37 F3 1.330(3) . ? C37 F1 1.334(3) . ? C37 F2 1.335(2) . ? C37 S1 1.819(2) . ? C38 F4 1.331(3) . ? C38 F5 1.335(3) . ? C38 F6 1.343(2) . ? C38 S2 1.822(2) . ? N1 Fe1 2.2151(16) . ? N2 Fe1 2.1176(17) . ? N3 Fe1 2.1999(15) . ? N4 Fe1 2.1681(16) . ? N5 Fe2 2.2577(15) . ? N6 Fe2 2.1235(16) . ? N7 Fe2 2.1673(16) . ? N8 Fe2 2.1439(17) . ? O1 Fe2 1.7965(13) . ? O1 Fe1 1.8254(13) . ? O2 Mo1 1.8203(13) . ? O2 Fe1 1.9248(14) . ? O3 Mo1 1.7988(14) . ? O3 Fe2 1.9678(14) . ? O4 Mo1 1.7235(15) . ? O5 Mo1 1.7242(15) . ? O6 S1 1.4436(17) . ? O7 S1 1.4403(17) . ? O8 S1 1.4377(17) . ? O9 S2 1.4354(15) . ? O10 S2 1.4437(16) . ? O11 S2 1.4391(17) . ? 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 N1 C1 C2 109.81(16) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N2 C2 C3 121.37(19) . . ? N2 C2 C1 115.81(17) . . ? C3 C2 C1 122.79(18) . . ? C2 C3 C4 118.8(2) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 119.65(19) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C6 C5 C4 118.3(2) . . ? C6 C5 H5 120.8 . . ? C4 C5 H5 120.8 . . ? N2 C6 C5 122.1(2) . . ? N2 C6 H6 118.9 . . ? C5 C6 H6 118.9 . . ? N1 C7 C8 112.88(15) . . ? N1 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N1 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? N3 C8 C9 121.91(18) . . ? N3 C8 C7 116.14(16) . . ? C9 C8 C7 121.88(17) . . ? C10 C9 C8 118.49(19) . . ? C10 C9 H9 120.8 . . ? C8 C9 H9 120.8 . . ? C9 C10 C11 119.49(19) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C12 C11 C10 118.8(2) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? N3 C12 C11 122.03(19) . . ? N3 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? N1 C13 C14 109.22(16) . . ? N1 C13 H13A 109.8 . . ? C14 C13 H13A 109.8 . . ? N1 C13 H13B 109.8 . . ? C14 C13 H13B 109.8 . . ? H13A C13 H13B 108.3 . . ? N4 C14 C15 121.93(19) . . ? N4 C14 C13 115.47(17) . . ? C15 C14 C13 122.60(18) . . ? C16 C15 C14 119.0(2) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C17 C16 C15 119.4(2) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 118.5(2) . . ? C16 C17 H17 120.7 . . ? C18 C17 H17 120.7 . . ? N4 C18 C17 122.33(19) . . ? N4 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? N5 C19 C20 111.94(15) . . ? N5 C19 H19A 109.2 . . ? C20 C19 H19A 109.2 . . ? N5 C19 H19B 109.2 . . ? C20 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? N6 C20 C21 121.06(19) . . ? N6 C20 C19 116.52(18) . . ? C21 C20 C19 122.26(18) . . ? C20 C21 C22 119.32(19) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C23 C22 C21 119.6(2) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 C22 118.03(19) . . ? C24 C23 H23 121.0 . . ? C22 C23 H23 121.0 . . ? N6 C24 C23 122.81(18) . . ? N6 C24 H24 118.6 . . ? C23 C24 H24 118.6 . . ? N5 C25 C26 113.33(15) . . ? N5 C25 H25A 108.9 . . ? C26 C25 H25A 108.9 . . ? N5 C25 H25B 108.9 . . ? C26 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? N7 C26 C27 122.05(18) . . ? N7 C26 C25 116.82(17) . . ? C27 C26 C25 121.07(17) . . ? C28 C27 C26 119.26(19) . . ? C28 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? C27 C28 C29 119.0(2) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? C30 C29 C28 118.5(2) . . ? C30 C29 H29 120.8 . . ? C28 C29 H29 120.8 . . ? N7 C30 C29 122.90(19) . . ? N7 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? N5 C31 C32 110.53(16) . . ? N5 C31 H31A 109.5 . . ? C32 C31 H31A 109.5 . . ? N5 C31 H31B 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? N8 C32 C33 121.6(2) . . ? N8 C32 C31 116.50(17) . . ? C33 C32 C31 121.84(19) . . ? C34 C33 C32 119.2(2) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 C35 119.4(2) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? C36 C35 C34 118.2(2) . . ? C36 C35 H35 120.9 . . ? C34 C35 H35 120.9 . . ? N8 C36 C35 122.7(2) . . ? N8 C36 H36 118.7 . . ? C35 C36 H36 118.7 . . ? F3 C37 F1 107.83(18) . . ? F3 C37 F2 107.81(17) . . ? F1 C37 F2 107.20(18) . . ? F3 C37 S1 111.47(15) . . ? F1 C37 S1 111.27(14) . . ? F2 C37 S1 111.07(15) . . ? F4 C38 F5 108.66(17) . . ? F4 C38 F6 107.05(17) . . ? F5 C38 F6 107.05(19) . . ? F4 C38 S2 111.26(16) . . ? F5 C38 S2 111.94(14) . . ? F6 C38 S2 110.67(14) . . ? C1 N1 C13 112.60(15) . . ? C1 N1 C7 110.69(15) . . ? C13 N1 C7 110.93(15) . . ? C1 N1 Fe1 105.80(11) . . ? C13 N1 Fe1 105.44(11) . . ? C7 N1 Fe1 111.15(11) . . ? C6 N2 C2 119.60(17) . . ? C6 N2 Fe1 124.37(14) . . ? C2 N2 Fe1 115.81(13) . . ? C12 N3 C8 118.99(17) . . ? C12 N3 Fe1 123.47(13) . . ? C8 N3 Fe1 113.89(12) . . ? C18 N4 C14 118.85(17) . . ? C18 N4 Fe1 125.91(14) . . ? C14 N4 Fe1 114.97(13) . . ? C31 N5 C25 110.09(15) . . ? C31 N5 C19 112.16(15) . . ? C25 N5 C19 112.09(16) . . ? C31 N5 Fe2 104.50(11) . . ? C25 N5 Fe2 110.09(11) . . ? C19 N5 Fe2 107.59(11) . . ? C20 N6 C24 119.15(17) . . ? C20 N6 Fe2 117.62(13) . . ? C24 N6 Fe2 123.20(13) . . ? C30 N7 C26 118.29(17) . . ? C30 N7 Fe2 123.43(13) . . ? C26 N7 Fe2 117.42(12) . . ? C36 N8 C32 118.85(18) . . ? C36 N8 Fe2 125.19(13) . . ? C32 N8 Fe2 114.94(13) . . ? Fe2 O1 Fe1 141.56(8) . . ? Mo1 O2 Fe1 132.67(8) . . ? Mo1 O3 Fe2 131.89(7) . . ? O8 S1 O7 115.54(11) . . ? O8 S1 O6 114.88(11) . . ? O7 S1 O6 114.90(11) . . ? O8 S1 C37 103.61(10) . . ? O7 S1 C37 102.71(10) . . ? O6 S1 C37 102.61(10) . . ? O9 S2 O11 115.30(10) . . ? O9 S2 O10 114.71(9) . . ? O11 S2 O10 114.90(11) . . ? O9 S2 C38 104.18(10) . . ? O11 S2 C38 103.13(10) . . ? O10 S2 C38 102.19(10) . . ? O1 Fe1 O2 99.62(6) . . ? O1 Fe1 N2 94.69(6) . . ? O2 Fe1 N2 103.19(6) . . ? O1 Fe1 N4 95.39(6) . . ? O2 Fe1 N4 101.94(6) . . ? N2 Fe1 N4 150.88(6) . . ? O1 Fe1 N3 172.10(6) . . ? O2 Fe1 N3 87.52(6) . . ? N2 Fe1 N3 86.91(6) . . ? N4 Fe1 N3 79.71(6) . . ? O1 Fe1 N1 95.07(6) . . ? O2 Fe1 N1 165.30(6) . . ? N2 Fe1 N1 75.92(6) . . ? N4 Fe1 N1 76.03(6) . . ? N3 Fe1 N1 77.79(6) . . ? O1 Fe2 O3 101.05(6) . . ? O1 Fe2 N6 102.52(6) . . ? O3 Fe2 N6 89.32(6) . . ? O1 Fe2 N8 105.19(6) . . ? O3 Fe2 N8 86.68(6) . . ? N6 Fe2 N8 152.26(6) . . ? O1 Fe2 N7 95.84(6) . . ? O3 Fe2 N7 162.86(6) . . ? N6 Fe2 N7 84.18(6) . . ? N8 Fe2 N7 91.72(6) . . ? O1 Fe2 N5 172.84(6) . . ? O3 Fe2 N5 86.11(6) . . ? N6 Fe2 N5 77.29(6) . . ? N8 Fe2 N5 75.06(6) . . ? N7 Fe2 N5 77.00(6) . . ? O4 Mo1 O5 108.47(8) . . ? O4 Mo1 O3 112.01(7) . . ? O5 Mo1 O3 107.92(7) . . ? O4 Mo1 O2 111.78(7) . . ? O5 Mo1 O2 109.98(7) . . ? O3 Mo1 O2 106.62(6) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.662 _refine_diff_density_min -1.301 _refine_diff_density_rms 0.089 _database_code_depnum_ccdc_archive 'CCDC 937040'