# Copyright The Royal Society of Chemistry, 1998 #----------------------------------------------------------------------- # CIF data for paper No. 8/06161K # # "Coupling Mo2n+ units via dicarboxylate bridges" # Authors: F. Albert Cotton, Chun Lin, Carlos A. Murillo # # J.Chem.Soc. Dalton Trans. submitted 31 July 1998 #----------------------------------------------------------------------- data_CMPD_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety [Mo2(p-MeOform)3]2(C2O4)(2CH2Cl2) _chemical_formula_sum 'C94 H94 Cl4 Mo4 N12 O16' _chemical_formula_weight 2173.37 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 13.998(2) _cell_length_b 17.441(3) _cell_length_c 20.229(1) _cell_angle_alpha 90.00 _cell_angle_beta 97.40(1) _cell_angle_gamma 90.00 _cell_volume 4898(1) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 250 _cell_measurement_theta_min 9.0 _cell_measurement_theta_max 20.8 _exptl_crystal_description cubic-shape _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2212 _exptl_absorpt_coefficient_mu 0.678 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.705 _exptl_absorpt_correction_T_max 0.844 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Nonius FAST area detector' _diffrn_measurement_method 'Ellipsoid-mask fitting' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'None (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18986 _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 22.57 _reflns_number_total 6356 _reflns_number_obs 5571 _reflns_threshold_expression >2sigma(I) _computing_data_collection MADNES _computing_cell_refinement MADNES _computing_data_reduction PROCOR _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0480P)^2^+26.2839P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6356 _refine_ls_number_parameters 596 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0620 _refine_ls_R_factor_obs 0.0524 _refine_ls_wR_factor_all 0.1292 _refine_ls_wR_factor_obs 0.1209 _refine_ls_goodness_of_fit_all 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.93962(3) 0.56590(3) 0.16091(2) 0.02113(16) Uani 1 d . . . Mo2 Mo 0.81082(3) 0.54842(3) 0.09810(2) 0.02147(16) Uani 1 d . . . N1 N 0.9583(3) 0.6799(3) 0.1272(2) 0.0237(10) Uani 1 d . . . N2 N 0.8145(3) 0.6636(3) 0.0600(2) 0.0246(10) Uani 1 d . . . N3 N 0.8647(3) 0.5997(3) 0.2418(2) 0.0246(10) Uani 1 d . . . N4 N 0.7232(3) 0.5753(2) 0.1739(2) 0.0221(10) Uani 1 d . . . N5 N 0.9517(3) 0.4500(2) 0.1923(2) 0.0258(11) Uani 1 d . . . N6 N 0.8145(3) 0.4268(3) 0.1202(2) 0.0241(10) Uani 1 d . . . C1 C 0.8921(4) 0.7055(3) 0.0800(3) 0.0256(13) Uani 1 d . . . H1A H 0.8998 0.7536 0.0604 0.031 Uiso 1 calc R . . C2 C 0.7698(4) 0.5961(3) 0.2329(3) 0.0237(12) Uani 1 d . . . H2A H 0.7349 0.6081 0.2682 0.028 Uiso 1 calc R . . C3 C 0.8885(4) 0.4018(3) 0.1619(3) 0.0278(13) Uani 1 d . . . H3A H 0.8960 0.3489 0.1699 0.033 Uiso 1 calc R . . C4 C 0.9734(4) 0.5140(3) 0.0278(3) 0.0231(12) Uani 1 d . . . O7 O 1.0216(3) 0.5306(2) 0.08368(17) 0.0231(8) Uani 1 d . . . O8 O 0.8825(3) 0.5174(2) 0.01618(17) 0.0253(9) Uani 1 d . . . O1 O 1.3010(3) 0.8355(2) 0.2132(2) 0.0347(10) Uani 1 d . . . C11 C 1.0432(4) 0.7239(3) 0.1479(2) 0.0223(12) Uani 1 d . . . C12 C 1.0427(4) 0.8030(3) 0.1545(3) 0.0278(13) Uani 1 d . . . H12A H 0.9847 0.8302 0.1447 0.033 Uiso 1 calc R . . C13 C 1.1277(4) 0.8421(3) 0.1755(3) 0.0290(13) Uani 1 d . . . H13A H 1.1271 0.8958 0.1790 0.035 Uiso 1 calc R . . C14 C 1.2135(4) 0.8026(3) 0.1915(3) 0.0259(13) Uani 1 d . . . C15 C 1.2137(4) 0.7234(3) 0.1851(3) 0.0325(14) Uani 1 d . . . H15A H 1.2716 0.6961 0.1956 0.039 Uiso 1 calc R . . C16 C 1.1299(4) 0.6846(3) 0.1634(3) 0.0313(14) Uani 1 d . . . H16A H 1.1312 0.6309 0.1590 0.038 Uiso 1 calc R . . C17 C 1.3040(5) 0.9168(4) 0.2181(4) 0.0437(17) Uani 1 d . . . H17A H 1.3692 0.9331 0.2338 0.066 Uiso 1 calc R . . H17B H 1.2611 0.9337 0.2491 0.066 Uiso 1 calc R . . H17C H 1.2838 0.9390 0.1746 0.066 Uiso 1 calc R . . O2 O 0.5940(4) 0.7379(3) -0.1819(3) 0.081(2) Uani 1 d . . . C21 C 0.7560(4) 0.6865(3) 0.0006(3) 0.0237(12) Uani 1 d . . . C22 C 0.7956(5) 0.7206(4) -0.0524(3) 0.0392(16) Uani 1 d . . . H22A H 0.8619 0.7317 -0.0475 0.047 Uiso 1 calc R . . C23 C 0.7395(5) 0.7381(4) -0.1115(3) 0.0495(19) Uani 1 d . . . H23A H 0.7671 0.7614 -0.1464 0.059 Uiso 1 calc R . . C24 C 0.6428(5) 0.7212(4) -0.1190(3) 0.0440(17) Uani 1 d . . . C25 C 0.6020(4) 0.6886(3) -0.0682(3) 0.0365(15) Uani 1 d . . . H25A H 0.5356 0.6780 -0.0735 0.044 Uiso 1 calc R . . C26 C 0.6591(4) 0.6709(3) -0.0083(3) 0.0311(14) Uani 1 d . . . H26A H 0.6307 0.6479 0.0264 0.037 Uiso 1 calc R . . C27 C 0.5100(5) 0.7009(5) -0.2022(4) 0.060(2) Uani 1 d . . . H27A H 0.4844 0.7182 -0.2465 0.090 Uiso 1 calc R . . H27B H 0.4639 0.7120 -0.1715 0.090 Uiso 1 calc R . . H27C H 0.5215 0.6461 -0.2029 0.090 Uiso 1 calc R . . O3 O 1.0561(4) 0.6535(4) 0.4964(2) 0.0709(18) Uani 1 d . . . C31 C 0.9113(4) 0.6153(3) 0.3075(3) 0.0247(13) Uani 1 d . . . C32 C 0.9925(4) 0.6618(3) 0.3150(3) 0.0279(13) Uani 1 d . . . H32A H 1.0133 0.6846 0.2772 0.033 Uiso 1 calc R . . C33 C 1.0431(5) 0.6749(4) 0.3773(3) 0.0399(16) Uani 1 d . . . H33A H 1.0984 0.7060 0.3819 0.048 Uiso 1 calc R . . C34 C 1.0118(5) 0.6421(4) 0.4328(3) 0.0414(17) Uani 1 d . . . C35 C 0.9320(5) 0.5958(4) 0.4256(3) 0.0470(18) Uani 1 d . . . H35A H 0.9109 0.5733 0.4634 0.056 Uiso 1 calc R . . C36 C 0.8824(4) 0.5820(4) 0.3631(3) 0.0348(15) Uani 1 d . . . H36A H 0.8284 0.5495 0.3587 0.042 Uiso 1 calc R . . C37 C 1.1411(7) 0.6997(8) 0.5039(4) 0.109(5) Uani 1 d . . . H37A H 1.1660 0.7038 0.5508 0.163 Uiso 1 calc R . . H37B H 1.1258 0.7504 0.4859 0.163 Uiso 1 calc R . . H37C H 1.1893 0.6762 0.4800 0.163 Uiso 1 calc R . . O4 O 0.3219(3) 0.5527(3) 0.1566(3) 0.0619(15) Uani 1 d . . . C41 C 0.6208(4) 0.5717(3) 0.1679(3) 0.0238(12) Uani 1 d . . . C42 C 0.5720(4) 0.5180(3) 0.1261(3) 0.0336(14) Uani 1 d . . . H42A H 0.6073 0.4862 0.1006 0.040 Uiso 1 calc R . . C43 C 0.4726(4) 0.5096(4) 0.1204(3) 0.0396(16) Uani 1 d . . . H43A H 0.4414 0.4729 0.0911 0.048 Uiso 1 calc R . . C44 C 0.4205(4) 0.5551(4) 0.1576(3) 0.0397(16) Uani 1 d . . . C45 C 0.4679(5) 0.6103(4) 0.1986(4) 0.0509(19) Uani 1 d . . . H45A H 0.4323 0.6424 0.2236 0.061 Uiso 1 calc R . . C46 C 0.5667(4) 0.6193(4) 0.2033(3) 0.0400(16) Uani 1 d . . . H46A H 0.5973 0.6579 0.2306 0.048 Uiso 1 calc R . . C47 C 0.2745(5) 0.4841(4) 0.1374(4) 0.060(2) Uani 1 d . . . H47A H 0.2059 0.4902 0.1389 0.091 Uiso 1 calc R . . H47B H 0.2991 0.4434 0.1677 0.091 Uiso 1 calc R . . H47C H 0.2856 0.4710 0.0924 0.091 Uiso 1 calc R . . O5 O 1.2734(4) 0.3496(3) 0.3637(3) 0.0760(17) Uani 1 d . . . C51 C 1.0361(4) 0.4219(3) 0.2323(3) 0.0270(13) Uani 1 d . . . C52 C 1.0736(5) 0.4641(4) 0.2881(3) 0.0400(16) Uani 1 d . . . H52A H 1.0441 0.5106 0.2974 0.048 Uiso 1 calc R . . C53 C 1.1526(5) 0.4395(4) 0.3297(4) 0.0506(19) Uani 1 d . . . H53A H 1.1763 0.4689 0.3671 0.061 Uiso 1 calc R . . C54 C 1.1976(5) 0.3714(4) 0.3167(4) 0.0473(18) Uani 1 d . . . C55 C 1.1641(5) 0.3296(4) 0.2615(4) 0.0460(17) Uani 1 d . . . H55A H 1.1945 0.2835 0.2525 0.055 Uiso 1 calc R . . C56 C 1.0844(5) 0.3556(4) 0.2184(3) 0.0434(17) Uani 1 d . . . H56A H 1.0633 0.3277 0.1795 0.052 Uiso 1 calc R . . C57 C 1.3198(7) 0.2853(6) 0.3513(5) 0.093(3) Uani 1 d . . . H57A H 1.3711 0.2758 0.3873 0.140 Uiso 1 calc R . . H57B H 1.3469 0.2907 0.3098 0.140 Uiso 1 calc R . . H57C H 1.2750 0.2426 0.3478 0.140 Uiso 1 calc R . . O6 O 0.5793(4) 0.2010(3) -0.0137(3) 0.0599(14) Uani 1 d . . . C61 C 0.7512(4) 0.3704(3) 0.0867(3) 0.0274(13) Uani 1 d . . . C62 C 0.7211(5) 0.3783(4) 0.0192(3) 0.0367(15) Uani 1 d . . . H62A H 0.7405 0.4215 -0.0034 0.044 Uiso 1 calc R . . C63 C 0.6631(5) 0.3238(4) -0.0154(3) 0.0443(17) Uani 1 d . . . H63A H 0.6429 0.3306 -0.0612 0.053 Uiso 1 calc R . . C64 C 0.6346(4) 0.2601(4) 0.0161(3) 0.0384(16) Uani 1 d . . . C65 C 0.6629(5) 0.2520(4) 0.0837(4) 0.0461(18) Uani 1 d . . . H65A H 0.6433 0.2086 0.1060 0.055 Uiso 1 calc R . . C66 C 0.7197(5) 0.3070(3) 0.1190(3) 0.0370(15) Uani 1 d . . . H66A H 0.7370 0.3013 0.1652 0.044 Uiso 1 calc R . . C67 C 0.5720(7) 0.1965(6) -0.0838(4) 0.085(3) Uani 1 d . . . H67A H 0.5317 0.1532 -0.0993 0.127 Uiso 1 calc R . . H67B H 0.6357 0.1898 -0.0970 0.127 Uiso 1 calc R . . H67C H 0.5435 0.2433 -0.1032 0.127 Uiso 1 calc R . . C1S C 0.6397(17) 0.9106(13) -0.0331(11) 0.121(7) Uiso 0.594(5) d PD A 1 Cl1S Cl 0.5778(8) 0.9175(5) -0.1136(4) 0.172(2) Uani 0.594(5) d PD A 1 Cl2S Cl 0.7039(7) 0.9950(5) -0.0147(4) 0.172(2) Uani 0.594(5) d PD A 1 C2S C 0.515(2) 0.925(2) -0.085(2) 0.121(7) Uiso 0.272(5) d PD B 2 Cl3S Cl 0.4387(17) 0.9814(11) -0.1374(8) 0.172(2) Uani 0.272(5) d PD B 2 Cl4S Cl 0.6268(15) 0.9649(11) -0.0684(8) 0.172(2) Uani 0.272(5) d PD B 2 C3S C 0.408(6) 0.961(5) -0.144(4) 0.121(7) Uiso 0.134(5) d PD C 3 Cl5S Cl 0.430(3) 1.0379(18) -0.1952(15) 0.172(2) Uani 0.134(5) d PD C 3 Cl6S Cl 0.304(3) 0.9146(18) -0.1774(15) 0.172(2) Uani 0.134(5) d PD C 3 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 0.0185(3) 0.0258(3) 0.0182(3) -0.00209(19) -0.00112(19) -0.00143(19) Mo2 0.0182(3) 0.0269(3) 0.0186(3) -0.0028(2) -0.0004(2) -0.0021(2) N1 0.019(2) 0.027(3) 0.023(2) 0.001(2) -0.002(2) -0.003(2) N2 0.023(3) 0.028(3) 0.022(2) 0.001(2) -0.003(2) -0.002(2) N3 0.025(3) 0.025(3) 0.023(3) -0.001(2) 0.002(2) 0.003(2) N4 0.017(2) 0.024(2) 0.024(3) -0.0007(19) 0.000(2) -0.0036(19) N5 0.028(3) 0.023(2) 0.025(3) -0.002(2) 0.001(2) -0.005(2) N6 0.022(3) 0.030(3) 0.019(2) -0.004(2) 0.000(2) 0.001(2) C1 0.024(3) 0.029(3) 0.023(3) 0.001(2) 0.002(3) -0.004(3) C2 0.021(3) 0.028(3) 0.021(3) -0.002(2) 0.003(2) 0.000(2) C3 0.033(3) 0.019(3) 0.031(3) -0.001(3) 0.005(3) 0.001(3) C4 0.026(3) 0.023(3) 0.020(3) 0.001(2) 0.002(2) -0.006(2) O7 0.020(2) 0.030(2) 0.019(2) -0.0041(16) -0.0006(16) -0.0022(16) O8 0.021(2) 0.033(2) 0.022(2) -0.0027(17) 0.0027(16) -0.0007(17) O1 0.026(2) 0.037(2) 0.038(2) -0.0088(19) -0.0099(18) -0.0055(19) C11 0.022(3) 0.026(3) 0.017(3) -0.002(2) -0.002(2) -0.006(2) C12 0.024(3) 0.032(3) 0.027(3) -0.006(3) -0.001(2) 0.001(3) C13 0.031(3) 0.024(3) 0.032(3) -0.006(3) 0.002(3) -0.007(3) C14 0.023(3) 0.032(3) 0.021(3) -0.001(2) -0.005(2) -0.003(3) C15 0.024(3) 0.029(3) 0.042(4) 0.004(3) -0.008(3) 0.005(3) C16 0.025(3) 0.025(3) 0.042(4) -0.002(3) -0.004(3) -0.002(3) C17 0.032(4) 0.037(4) 0.058(4) -0.010(3) -0.007(3) -0.011(3) O2 0.082(4) 0.083(4) 0.064(4) 0.042(3) -0.046(3) -0.036(3) C21 0.022(3) 0.020(3) 0.029(3) -0.005(2) 0.001(2) -0.002(2) C22 0.027(3) 0.050(4) 0.038(4) 0.007(3) -0.002(3) -0.006(3) C23 0.048(4) 0.064(5) 0.032(4) 0.018(3) -0.012(3) -0.019(4) C24 0.047(4) 0.038(4) 0.039(4) 0.015(3) -0.021(3) -0.006(3) C25 0.023(3) 0.037(4) 0.046(4) -0.004(3) -0.009(3) -0.003(3) C26 0.029(4) 0.033(3) 0.030(3) -0.001(3) 0.000(3) 0.000(3) C27 0.048(5) 0.081(6) 0.045(4) 0.012(4) -0.015(4) -0.017(4) O3 0.061(3) 0.127(5) 0.022(2) -0.003(3) -0.005(2) -0.049(3) C31 0.025(3) 0.030(3) 0.020(3) -0.005(2) 0.003(2) 0.002(3) C32 0.032(3) 0.034(3) 0.016(3) -0.002(2) 0.000(2) -0.009(3) C33 0.035(4) 0.053(4) 0.032(4) -0.006(3) 0.004(3) -0.020(3) C34 0.034(4) 0.067(5) 0.021(3) -0.006(3) -0.003(3) -0.016(3) C35 0.044(4) 0.071(5) 0.026(4) 0.003(3) 0.007(3) -0.013(4) C36 0.029(3) 0.050(4) 0.025(3) -0.006(3) 0.001(3) -0.013(3) C37 0.068(6) 0.221(14) 0.035(5) -0.014(6) -0.004(4) -0.083(8) O4 0.023(3) 0.052(3) 0.109(5) -0.024(3) 0.001(3) -0.001(2) C41 0.024(3) 0.024(3) 0.023(3) 0.001(2) 0.000(2) -0.003(2) C42 0.025(3) 0.036(3) 0.039(4) -0.010(3) 0.002(3) -0.001(3) C43 0.031(4) 0.034(4) 0.051(4) -0.010(3) -0.007(3) -0.005(3) C44 0.023(3) 0.042(4) 0.053(4) -0.002(3) -0.003(3) 0.001(3) C45 0.033(4) 0.051(4) 0.068(5) -0.026(4) 0.003(3) 0.005(3) C46 0.028(4) 0.040(4) 0.050(4) -0.017(3) -0.004(3) 0.004(3) C47 0.026(4) 0.060(5) 0.094(6) -0.014(4) 0.002(4) -0.006(3) O5 0.053(3) 0.063(4) 0.104(5) 0.010(3) -0.023(3) 0.018(3) C51 0.022(3) 0.024(3) 0.033(3) 0.006(3) -0.002(3) -0.003(2) C52 0.037(4) 0.030(3) 0.047(4) 0.001(3) -0.013(3) 0.000(3) C53 0.048(4) 0.041(4) 0.055(5) -0.005(3) -0.022(4) -0.002(3) C54 0.031(4) 0.043(4) 0.062(5) 0.009(4) -0.019(3) 0.002(3) C55 0.033(4) 0.039(4) 0.066(5) 0.005(4) 0.005(3) 0.011(3) C56 0.037(4) 0.054(4) 0.039(4) -0.005(3) 0.002(3) 0.006(3) C57 0.071(7) 0.103(8) 0.103(8) 0.022(7) 0.002(6) 0.014(6) O6 0.059(3) 0.062(3) 0.059(3) -0.028(3) 0.010(3) -0.027(3) C61 0.025(3) 0.025(3) 0.031(3) -0.006(3) 0.001(3) -0.001(2) C62 0.041(4) 0.033(3) 0.032(4) 0.002(3) -0.009(3) -0.001(3) C63 0.048(4) 0.045(4) 0.036(4) -0.005(3) -0.008(3) -0.006(3) C64 0.029(3) 0.043(4) 0.044(4) -0.022(3) 0.008(3) -0.011(3) C65 0.046(4) 0.042(4) 0.054(5) -0.014(3) 0.018(3) -0.018(3) C66 0.040(4) 0.039(4) 0.035(4) -0.007(3) 0.013(3) -0.010(3) C67 0.090(7) 0.087(7) 0.072(6) -0.033(5) -0.012(5) -0.028(6) Cl1S 0.256(7) 0.148(4) 0.112(3) 0.005(3) 0.017(4) 0.024(4) Cl2S 0.256(7) 0.148(4) 0.112(3) 0.005(3) 0.017(4) 0.024(4) Cl3S 0.256(7) 0.148(4) 0.112(3) 0.005(3) 0.017(4) 0.024(4) Cl4S 0.256(7) 0.148(4) 0.112(3) 0.005(3) 0.017(4) 0.024(4) Cl5S 0.256(7) 0.148(4) 0.112(3) 0.005(3) 0.017(4) 0.024(4) Cl6S 0.256(7) 0.148(4) 0.112(3) 0.005(3) 0.017(4) 0.024(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 Mo2 2.0900(7) . Y Mo1 N5 2.119(4) . Y Mo1 N1 2.130(4) . Y Mo1 N3 2.137(4) . Y Mo1 O7 2.145(3) . Y Mo2 O8 2.115(3) . Y Mo2 N4 2.135(4) . Y Mo2 N2 2.155(4) . Y Mo2 N6 2.168(5) . Y N1 C1 1.320(7) . ? N1 C11 1.431(7) . ? N2 C1 1.327(7) . ? N2 C21 1.421(7) . ? N3 C2 1.318(7) . ? N3 C31 1.430(7) . ? N4 C2 1.335(7) . ? N4 C41 1.425(7) . ? N5 C3 1.314(7) . ? N5 C51 1.431(7) . ? N6 C3 1.323(7) . ? N6 C61 1.435(7) . ? C4 O8 1.266(6) . ? C4 O7 1.272(6) . ? C4 C4 1.508(11) 3_765 ? O1 C14 1.373(7) . ? O1 C17 1.421(7) . ? C11 C12 1.385(8) . ? C11 C16 1.395(8) . ? C12 C13 1.391(8) . ? C13 C14 1.386(8) . ? C14 C15 1.386(8) . ? C15 C16 1.377(8) . ? O2 C27 1.357(8) . ? O2 C24 1.395(8) . ? C21 C26 1.372(8) . ? C21 C22 1.402(8) . ? C22 C23 1.378(9) . ? C23 C24 1.373(10) . ? C24 C25 1.364(9) . ? C25 C26 1.397(8) . ? O3 C34 1.371(7) . ? O3 C37 1.429(9) . ? C31 C36 1.372(8) . ? C31 C32 1.389(8) . ? C32 C33 1.384(8) . ? C33 C34 1.380(9) . ? C34 C35 1.370(9) . ? C35 C36 1.382(9) . ? O4 C44 1.378(8) . ? O4 C47 1.400(8) . ? C41 C42 1.382(8) . ? C41 C46 1.383(8) . ? C42 C43 1.390(8) . ? C43 C44 1.368(9) . ? C44 C45 1.383(9) . ? C45 C46 1.384(9) . ? O5 C57 1.335(11) . ? O5 C54 1.383(8) . ? C51 C56 1.386(9) . ? C51 C52 1.393(8) . ? C52 C53 1.369(9) . ? C53 C54 1.385(10) . ? C54 C55 1.365(10) . ? C55 C56 1.401(9) . ? O6 C64 1.379(7) . ? O6 C67 1.409(10) . ? C61 C62 1.382(8) . ? C61 C66 1.385(8) . ? C62 C63 1.382(9) . ? C63 C64 1.367(9) . ? C64 C65 1.380(10) . ? C65 C66 1.384(9) . ? C1S Cl2S 1.74(2) . ? C1S Cl1S 1.75(2) . ? C2S Cl4S 1.70(3) . ? C2S Cl3S 1.71(3) . ? C3S Cl6S 1.73(3) . ? C3S Cl5S 1.73(3) . ? 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 Mo2 Mo1 N5 94.13(13) . . Y Mo2 Mo1 N1 94.21(12) . . Y N5 Mo1 N1 168.12(17) . . Y Mo2 Mo1 N3 92.04(12) . . Y N5 Mo1 N3 93.53(17) . . Y N1 Mo1 N3 94.61(17) . . Y Mo2 Mo1 O7 90.91(9) . . Y N5 Mo1 O7 85.10(16) . . Y N1 Mo1 O7 86.32(15) . . Y N3 Mo1 O7 176.83(15) . . Y Mo1 Mo2 O8 93.13(10) . . Y Mo1 Mo2 N4 93.53(12) . . Y O8 Mo2 N4 173.24(15) . . Y Mo1 Mo2 N2 91.31(12) . . Y O8 Mo2 N2 85.57(15) . . Y N4 Mo2 N2 95.41(17) . . Y Mo1 Mo2 N6 91.24(12) . . Y O8 Mo2 N6 84.82(15) . . Y N4 Mo2 N6 93.90(16) . . Y N2 Mo2 N6 170.18(16) . . Y C1 N1 C11 120.7(5) . . ? C1 N1 Mo1 116.3(4) . . ? C11 N1 Mo1 122.6(3) . . ? C1 N2 C21 117.6(5) . . ? C1 N2 Mo2 117.4(4) . . ? C21 N2 Mo2 121.7(3) . . ? C2 N3 C31 117.9(4) . . ? C2 N3 Mo1 117.9(4) . . ? C31 N3 Mo1 123.7(3) . . ? C2 N4 C41 117.3(4) . . ? C2 N4 Mo2 116.3(3) . . ? C41 N4 Mo2 126.5(3) . . ? C3 N5 C51 120.2(5) . . ? C3 N5 Mo1 116.6(4) . . ? C51 N5 Mo1 121.6(3) . . ? C3 N6 C61 117.5(5) . . ? C3 N6 Mo2 116.7(4) . . ? C61 N6 Mo2 125.2(4) . . ? N1 C1 N2 120.3(5) . . ? N3 C2 N4 120.2(5) . . ? N5 C3 N6 120.8(5) . . ? O8 C4 O7 124.1(5) . . ? O8 C4 C4 117.2(6) . 3_765 ? O7 C4 C4 118.7(6) . 3_765 ? C4 O7 Mo1 116.1(3) . . ? C4 O8 Mo2 115.7(3) . . ? C14 O1 C17 117.2(5) . . ? C12 C11 C16 118.9(5) . . ? C12 C11 N1 123.2(5) . . ? C16 C11 N1 117.9(5) . . ? C11 C12 C13 120.2(5) . . ? C14 C13 C12 120.6(5) . . ? O1 C14 C15 115.7(5) . . ? O1 C14 C13 125.2(5) . . ? C15 C14 C13 119.1(5) . . ? C16 C15 C14 120.5(5) . . ? C15 C16 C11 120.7(5) . . ? C27 O2 C24 118.7(6) . . ? C26 C21 C22 117.7(5) . . ? C26 C21 N2 120.6(5) . . ? C22 C21 N2 121.6(5) . . ? C23 C22 C21 121.3(6) . . ? C24 C23 C22 119.5(6) . . ? C25 C24 C23 120.6(6) . . ? C25 C24 O2 124.8(6) . . ? C23 C24 O2 114.7(6) . . ? C24 C25 C26 119.8(6) . . ? C21 C26 C25 121.1(6) . . ? C34 O3 C37 116.8(5) . . ? C36 C31 C32 118.8(5) . . ? C36 C31 N3 122.3(5) . . ? C32 C31 N3 118.8(5) . . ? C33 C32 C31 120.8(5) . . ? C34 C33 C32 119.5(6) . . ? C35 C34 O3 116.7(6) . . ? C35 C34 C33 119.9(6) . . ? O3 C34 C33 123.4(6) . . ? C34 C35 C36 120.4(6) . . ? C31 C36 C35 120.6(6) . . ? C44 O4 C47 117.9(5) . . ? C42 C41 C46 117.6(5) . . ? C42 C41 N4 119.6(5) . . ? C46 C41 N4 122.8(5) . . ? C41 C42 C43 122.2(6) . . ? C44 C43 C42 119.4(6) . . ? C43 C44 O4 125.3(6) . . ? C43 C44 C45 119.1(6) . . ? O4 C44 C45 115.6(6) . . ? C44 C45 C46 121.2(6) . . ? C41 C46 C45 120.4(6) . . ? C57 O5 C54 116.8(7) . . ? C56 C51 C52 117.6(6) . . ? C56 C51 N5 124.0(5) . . ? C52 C51 N5 118.4(5) . . ? C53 C52 C51 121.5(6) . . ? C52 C53 C54 120.3(6) . . ? C55 C54 O5 124.5(6) . . ? C55 C54 C53 119.7(6) . . ? O5 C54 C53 115.7(6) . . ? C54 C55 C56 120.0(6) . . ? C51 C56 C55 120.8(6) . . ? C64 O6 C67 116.5(6) . . ? C62 C61 C66 118.1(5) . . ? C62 C61 N6 119.2(5) . . ? C66 C61 N6 122.6(5) . . ? C61 C62 C63 121.1(6) . . ? C64 C63 C62 120.7(6) . . ? C63 C64 O6 125.7(6) . . ? C63 C64 C65 118.8(6) . . ? O6 C64 C65 115.6(6) . . ? C64 C65 C66 120.9(6) . . ? C65 C66 C61 120.4(6) . . ? Cl2S C1S Cl1S 108.8(13) . . ? Cl4S C2S Cl3S 112(2) . . ? Cl6S C3S Cl5S 110(2) . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 22.57 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 0.897 _refine_diff_density_min -0.561 _refine_diff_density_rms 0.103 #===END data_CMPD_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety '[Mo2(p-MeOform)3]2(O2CC6F4CO2)(2CH2Cl2)(C6H14)' _chemical_formula_sum 'C106 H108 Cl4 F4 Mo4 N12 O16' _chemical_formula_weight 2407.60 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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P(-1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.791(1) _cell_length_b 15.756(2) _cell_length_c 18.090(3) _cell_angle_alpha 76.65(1) _cell_angle_beta 79.61(1) _cell_angle_gamma 87.63(1) _cell_volume 2670.8(6) _cell_formula_units_Z 1 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 225 _cell_measurement_theta_min 9.0 _cell_measurement_theta_max 20.8 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1228 _exptl_absorpt_coefficient_mu 0.635 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.712 _exptl_absorpt_correction_T_max 0.895 _exptl_special_details ; Angle to L.S. plane (with approximate esd) = 30.43 ( 0.18 ) ; _diffrn_ambient_temperature 213(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 'Nonius FAST area detector' _diffrn_measurement_method 'Ellipsoid-mask fitting' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 'None (area detector data)' _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13247 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 22.53 _reflns_number_total 6664 _reflns_number_obs 5555 _reflns_threshold_expression >2sigma(I) _computing_data_collection MADNES _computing_cell_refinement MADNES _computing_data_reduction PROCOR _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens, 1990)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0860P)^2^+17.0794P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6664 _refine_ls_number_parameters 647 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0816 _refine_ls_R_factor_obs 0.0675 _refine_ls_wR_factor_all 0.1806 _refine_ls_wR_factor_obs 0.1663 _refine_ls_goodness_of_fit_all 1.036 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/esd_max 0.054 _refine_ls_shift/esd_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo -1.22525(6) -0.35361(4) 0.22792(4) 0.0360(2) Uani 1 d . . . Mo2 Mo -1.32398(6) -0.27308(4) 0.29835(4) 0.0360(2) Uani 1 d . . . N1 N -1.3915(6) -0.4476(4) 0.2690(3) 0.0361(14) Uani 1 d . . . N2 N -1.5008(6) -0.3557(4) 0.3416(3) 0.0373(14) Uani 1 d . . . N3 N -1.3093(6) -0.2864(4) 0.1313(3) 0.0384(14) Uani 1 d . . . N4 N -1.4156(6) -0.1966(4) 0.2072(4) 0.0383(15) Uani 1 d . . . N5 N -1.0423(6) -0.2739(4) 0.1956(4) 0.0410(15) Uani 1 d . . . N6 N -1.1476(6) -0.1897(4) 0.2761(4) 0.0425(15) Uani 1 d . . . O7 O -1.2321(5) -0.3462(3) 0.3938(3) 0.0362(11) Uani 1 d . . . O8 O -1.1240(5) -0.4280(3) 0.3161(3) 0.0353(11) Uani 1 d . . . C1 C -1.4960(7) -0.4315(5) 0.3214(4) 0.0362(17) Uani 1 d . . . H1A H -1.5660 -0.4734 0.3441 0.043 Uiso 1 calc R . . C2 C -1.3889(7) -0.2173(5) 0.1393(4) 0.0410(18) Uani 1 d . . . H2A H -1.4255 -0.1837 0.0972 0.049 Uiso 1 calc R . . C3 C -1.0358(8) -0.2098(5) 0.2311(5) 0.046(2) Uani 1 d . . . H3A H -0.9525 -0.1791 0.2242 0.055 Uiso 1 calc R . . C4 C -1.1478(7) -0.4056(4) 0.3798(4) 0.0329(16) Uani 1 d . . . C5 C -1.0719(7) -0.4532(4) 0.4413(4) 0.0363(17) Uani 1 d . . . C6 C -1.1266(7) -0.4654(5) 0.5192(4) 0.0358(17) Uani 1 d . . . C7 C -1.0595(7) -0.5098(5) 0.5754(4) 0.0358(17) Uani 1 d . . . F1 F -1.2539(4) -0.4342(3) 0.5419(3) 0.0498(11) Uani 1 d . . . F2 F -1.1236(4) -0.5199(3) 0.6493(2) 0.0485(11) Uani 1 d . . . O1 O -1.3923(9) -0.7746(4) 0.1988(5) 0.092(2) Uani 1 d . . . C11 C -1.3925(8) -0.5302(5) 0.2500(4) 0.0416(18) Uani 1 d . . . C12 C -1.5120(9) -0.5679(5) 0.2404(5) 0.050(2) Uani 1 d . . . H12A H -1.5968 -0.5377 0.2457 0.060 Uiso 1 calc R . . C13 C -1.5080(10) -0.6484(6) 0.2232(6) 0.062(2) Uani 1 d . . . H13A H -1.5897 -0.6727 0.2164 0.074 Uiso 1 calc R . . C14 C -1.3846(11) -0.6941(6) 0.2158(6) 0.063(3) Uani 1 d . . . C15 C -1.2637(11) -0.6572(6) 0.2229(6) 0.064(3) Uani 1 d . . . H15A H -1.1788 -0.6870 0.2161 0.077 Uiso 1 calc R . . C16 C -1.2684(9) -0.5765(5) 0.2402(5) 0.051(2) Uani 1 d . . . H16A H -1.1859 -0.5518 0.2454 0.061 Uiso 1 calc R . . C17 C -1.2713(15) -0.8251(8) 0.1966(9) 0.119(5) Uani 1 d . . . H17A H -1.2893 -0.8798 0.1842 0.178 Uiso 1 calc R . . H17B H -1.2425 -0.8368 0.2466 0.178 Uiso 1 calc R . . H17C H -1.1982 -0.7938 0.1575 0.178 Uiso 1 calc R . . O2 O -1.9195(9) -0.3299(6) 0.5917(6) 0.064(2) Uiso 0.720(11) d PD A 1 C27 C -2.0352(18) -0.2739(11) 0.5796(11) 0.090(5) Uiso 0.720(11) d PD A 1 H27A H -2.0993 -0.2788 0.6280 0.135 Uiso 0.720(11) calc PR A 1 H27B H -2.0819 -0.2907 0.5422 0.135 Uiso 0.720(11) calc PR A 1 H27C H -2.0032 -0.2141 0.5604 0.135 Uiso 0.720(11) calc PR A 1 O2' O -1.949(3) -0.2955(16) 0.5549(13) 0.064(2) Uiso 0.280(11) d PD A 2 C27' C -1.967(5) -0.310(3) 0.6366(18) 0.090(5) Uiso 0.280(11) d PD A 2 H27D H -2.0567 -0.2882 0.6563 0.135 Uiso 0.280(11) calc PR A 2 H27E H -1.8942 -0.2807 0.6508 0.135 Uiso 0.280(11) calc PR A 2 H27F H -1.9623 -0.3725 0.6586 0.135 Uiso 0.280(11) calc PR A 2 C21 C -1.6101(7) -0.3440(5) 0.4019(4) 0.0381(18) Uani 1 d . . . C22 C -1.6071(9) -0.3872(6) 0.4783(5) 0.052(2) Uani 1 d . . . H22A H -1.5307 -0.4230 0.4893 0.062 Uiso 1 calc R . . C23 C -1.7118(10) -0.3792(7) 0.5379(6) 0.066(3) Uani 1 d . . . H23A H -1.7076 -0.4102 0.5885 0.079 Uiso 1 calc R . . C24 C -1.8223(11) -0.3259(7) 0.5234(7) 0.072(3) Uani 1 d . . . C25 C -1.8271(9) -0.2790(7) 0.4482(8) 0.072(3) Uani 1 d . . . H25A H -1.9015 -0.2412 0.4379 0.086 Uiso 1 calc R . . C26 C -1.7201(8) -0.2892(5) 0.3889(6) 0.053(2) Uani 1 d . . . H26A H -1.7233 -0.2576 0.3384 0.063 Uiso 1 calc R . . O3 O -1.1095(8) -0.3521(5) -0.1606(4) 0.0751(19) Uani 1 d . . . C31 C -1.2618(8) -0.3027(5) 0.0563(4) 0.0413(18) Uani 1 d . . . C32 C -1.2323(9) -0.2361(6) -0.0109(5) 0.055(2) Uani 1 d . . . H32A H -1.2477 -0.1776 -0.0078 0.066 Uiso 1 calc R . . C33 C -1.1818(10) -0.2550(6) -0.0804(5) 0.063(3) Uani 1 d . . . H33A H -1.1632 -0.2095 -0.1247 0.076 Uiso 1 calc R . . C34 C -1.1577(9) -0.3400(6) -0.0863(5) 0.054(2) Uani 1 d . . . C35 C -1.1807(9) -0.4052(6) -0.0226(5) 0.056(2) Uani 1 d . . . H35A H -1.1612 -0.4631 -0.0264 0.067 Uiso 1 calc R . . C36 C -1.2336(9) -0.3869(6) 0.0494(5) 0.049(2) Uani 1 d . . . H36A H -1.2500 -0.4329 0.0935 0.059 Uiso 1 calc R . . C37 C -1.1074(12) -0.4389(7) -0.1704(6) 0.078(3) Uani 1 d . . . H37A H -1.0722 -0.4392 -0.2240 0.118 Uiso 1 calc R . . H37B H -1.2007 -0.4626 -0.1558 0.118 Uiso 1 calc R . . H37C H -1.0476 -0.4742 -0.1380 0.118 Uiso 1 calc R . . O4 O -1.7678(6) 0.0864(4) 0.2322(4) 0.0663(17) Uani 1 d . . . C41 C -1.5079(8) -0.1261(5) 0.2145(5) 0.0423(19) Uani 1 d . . . C42 C -1.6226(9) -0.1104(6) 0.1785(5) 0.058(2) Uani 1 d . . . H42A H -1.6426 -0.1484 0.1487 0.070 Uiso 1 calc R . . C43 C -1.7084(10) -0.0395(6) 0.1856(5) 0.060(2) Uani 1 d . . . H43A H -1.7855 -0.0291 0.1604 0.072 Uiso 1 calc R . . C44 C -1.6792(9) 0.0172(5) 0.2310(5) 0.054(2) Uani 1 d . . . C45 C -1.5699(10) -0.0008(6) 0.2701(6) 0.063(3) Uani 1 d . . . H45A H -1.5527 0.0349 0.3025 0.076 Uiso 1 calc R . . C46 C -1.4857(10) -0.0711(6) 0.2618(5) 0.057(2) Uani 1 d . . . H46A H -1.4108 -0.0826 0.2887 0.068 Uiso 1 calc R . . C47 C -1.7399(11) 0.1453(6) 0.2768(7) 0.078(3) Uani 1 d . . . H47A H -1.8084 0.1916 0.2740 0.117 Uiso 1 calc R . . H47B H -1.6480 0.1701 0.2567 0.117 Uiso 1 calc R . . H47C H -1.7444 0.1142 0.3302 0.117 Uiso 1 calc R . . O5 O -0.5545(6) -0.3936(5) 0.0415(4) 0.076(2) Uani 1 d . . . C51 C -0.9163(8) -0.3011(5) 0.1539(4) 0.0412(18) Uani 1 d . . . C52 C -0.8004(8) -0.3267(5) 0.1892(5) 0.049(2) Uani 1 d . . . H52A H -0.8048 -0.3245 0.2411 0.059 Uiso 1 calc R . . C56 C -0.9065(9) -0.3068(6) 0.0774(5) 0.057(2) Uani 1 d . . . H52B H -0.9827 -0.2900 0.0522 0.068 Uiso 1 calc R . . C53 C -0.6803(8) -0.3549(6) 0.1498(5) 0.052(2) Uani 1 d . . . H53A H -0.6027 -0.3698 0.1740 0.062 Uiso 1 calc R . . C55 C -0.7888(9) -0.3362(7) 0.0382(5) 0.062(2) Uani 1 d . . . H53C H -0.7847 -0.3397 -0.0133 0.074 Uiso 1 calc R . . C54 C -0.6745(8) -0.3613(6) 0.0744(5) 0.054(2) Uani 1 d . . . C57 C -0.5372(10) -0.3891(9) -0.0405(6) 0.085(3) Uani 1 d . . . H57A H -0.4481 -0.4139 -0.0577 0.128 Uiso 1 calc R . . H57B H -0.5409 -0.3287 -0.0681 0.128 Uiso 1 calc R . . H57C H -0.6109 -0.4217 -0.0506 0.128 Uiso 1 calc R . . O6 O -1.1256(8) 0.0672(5) 0.4424(5) 0.090(2) Uani 1 d . . . C61 C -1.1385(8) -0.1233(5) 0.3178(5) 0.045(2) Uani 1 d . . . C62 C -1.0786(10) -0.0438(6) 0.2850(6) 0.066(3) Uani 1 d . . . H62A H -1.0373 -0.0306 0.2326 0.079 Uiso 1 calc R . . C63 C -1.0787(11) 0.0189(6) 0.3297(8) 0.076(3) Uani 1 d . . . H63A H -1.0393 0.0741 0.3065 0.092 Uiso 1 calc R . . C64 C -1.1356(11) -0.0003(6) 0.4066(7) 0.070(3) Uani 1 d . . . C65 C -1.1961(11) -0.0770(6) 0.4387(7) 0.074(3) Uani 1 d . . . H65A H -1.2401 -0.0888 0.4907 0.089 Uiso 1 calc R . . C66 C -1.1950(10) -0.1397(6) 0.3964(6) 0.064(3) Uani 1 d . . . H66A H -1.2333 -0.1949 0.4211 0.077 Uiso 1 calc R . . C67 C -1.1854(14) 0.0479(8) 0.5244(9) 0.104(4) Uani 1 d . . . H67A H -1.1745 0.0981 0.5454 0.157 Uiso 1 calc R . . H67B H -1.1383 -0.0019 0.5513 0.157 Uiso 1 calc R . . H67C H -1.2834 0.0347 0.5310 0.157 Uiso 1 calc R . . C1S C -1.5594(17) -0.2038(11) 0.5718(9) 0.102(5) Uiso 0.864(5) d PD B 1 Cl1S Cl -1.5454(5) -0.1047(3) 0.5885(3) 0.1061(10) Uani 0.864(5) d PD B 1 Cl2S Cl -1.4131(5) -0.2663(3) 0.5736(3) 0.1061(10) Uani 0.864(5) d PD B 1 C1S' C -1.459(5) -0.189(4) 0.588(5) 0.102(5) Uiso 0.136(5) d PD B 2 Cl3S Cl -1.310(3) -0.2461(17) 0.5863(16) 0.1061(10) Uani 0.136(5) d PD B 2 Cl4S Cl -1.489(3) -0.0850(17) 0.5410(19) 0.1061(10) Uani 0.136(5) d PD B 2 C2S C -1.3101(15) 0.0243(9) 0.0398(9) 0.100 Uiso 0.92(2) d PD . . C3S C -1.186(2) -1.0003(13) 0.0649(12) 0.100 Uiso 0.67(3) d P . . C4S C -1.933(3) -0.018(2) 0.0080(18) 0.100 Uiso 0.45(2) d P . 1 Cl6S Cl -1.954(2) -0.0544(14) -0.0787(13) 0.100 Uiso 0.158(7) d P . 2 C5S C -1.396(3) 0.1120(13) 0.0376(16) 0.100 Uiso 0.49(2) d PD . . 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 0.0375(4) 0.0380(4) 0.0351(4) -0.0117(3) -0.0103(3) 0.0063(3) Mo2 0.0365(4) 0.0354(4) 0.0391(4) -0.0123(3) -0.0109(3) 0.0056(3) N1 0.039(3) 0.037(3) 0.037(3) -0.016(3) -0.010(3) 0.005(3) N2 0.038(3) 0.040(4) 0.038(4) -0.012(3) -0.014(3) 0.002(3) N3 0.041(3) 0.044(4) 0.031(3) -0.009(3) -0.010(3) 0.006(3) N4 0.039(3) 0.036(3) 0.042(4) -0.010(3) -0.012(3) 0.011(3) N5 0.037(3) 0.042(4) 0.044(4) -0.008(3) -0.010(3) 0.003(3) N6 0.041(4) 0.036(4) 0.052(4) -0.012(3) -0.009(3) 0.000(3) O7 0.039(3) 0.036(3) 0.037(3) -0.016(2) -0.010(2) 0.010(2) O8 0.037(3) 0.043(3) 0.031(3) -0.017(2) -0.011(2) 0.010(2) C1 0.035(4) 0.039(4) 0.037(4) -0.013(3) -0.005(3) -0.001(3) C2 0.037(4) 0.047(5) 0.038(5) -0.001(4) -0.016(4) 0.003(4) C3 0.037(4) 0.038(4) 0.060(5) -0.007(4) -0.007(4) -0.008(3) C4 0.035(4) 0.032(4) 0.033(4) -0.008(3) -0.006(3) -0.001(3) C5 0.040(4) 0.027(4) 0.045(5) -0.011(3) -0.011(4) 0.003(3) C6 0.029(4) 0.035(4) 0.048(5) -0.019(3) -0.007(4) 0.006(3) C7 0.039(4) 0.036(4) 0.035(4) -0.015(3) -0.004(4) 0.002(3) F1 0.041(2) 0.060(3) 0.049(3) -0.016(2) -0.010(2) 0.017(2) F2 0.044(2) 0.065(3) 0.037(3) -0.014(2) -0.007(2) 0.012(2) O1 0.123(6) 0.050(4) 0.116(6) -0.043(4) -0.027(5) 0.013(4) C11 0.052(5) 0.038(4) 0.036(4) -0.014(3) -0.006(4) 0.007(4) C12 0.050(5) 0.052(5) 0.051(5) -0.023(4) -0.006(4) 0.000(4) C13 0.069(6) 0.053(6) 0.074(7) -0.030(5) -0.017(5) -0.005(5) C14 0.091(7) 0.040(5) 0.066(6) -0.024(4) -0.018(5) 0.003(5) C15 0.073(6) 0.057(6) 0.066(6) -0.028(5) -0.009(5) 0.027(5) C16 0.053(5) 0.050(5) 0.055(5) -0.022(4) -0.008(4) 0.007(4) C17 0.139(12) 0.075(8) 0.154(14) -0.056(9) -0.022(10) 0.034(8) C21 0.035(4) 0.038(4) 0.047(5) -0.026(4) -0.003(4) -0.003(3) C22 0.051(5) 0.061(5) 0.051(5) -0.022(4) -0.012(4) -0.002(4) C23 0.058(6) 0.084(7) 0.062(6) -0.038(5) 0.001(5) -0.010(5) C24 0.069(7) 0.066(6) 0.083(8) -0.051(6) 0.033(6) -0.026(5) C25 0.038(5) 0.059(6) 0.131(11) -0.056(7) -0.008(6) 0.001(4) C26 0.042(5) 0.050(5) 0.076(6) -0.027(4) -0.018(4) 0.005(4) O3 0.093(5) 0.085(5) 0.050(4) -0.026(3) -0.006(4) 0.008(4) C31 0.041(4) 0.047(5) 0.039(5) -0.014(4) -0.013(4) 0.009(3) C32 0.068(6) 0.050(5) 0.048(5) -0.007(4) -0.019(5) 0.009(4) C33 0.078(6) 0.061(6) 0.040(5) 0.001(4) -0.003(5) 0.008(5) C34 0.057(5) 0.073(6) 0.033(5) -0.017(4) -0.008(4) 0.007(4) C35 0.065(6) 0.063(6) 0.045(5) -0.021(5) -0.015(4) 0.013(4) C36 0.054(5) 0.052(5) 0.041(5) -0.007(4) -0.013(4) 0.005(4) C37 0.089(8) 0.089(8) 0.061(6) -0.037(6) 0.003(6) 0.004(6) O4 0.061(4) 0.054(4) 0.089(5) -0.025(3) -0.017(3) 0.022(3) C41 0.042(4) 0.041(4) 0.046(5) -0.009(4) -0.018(4) 0.010(3) C42 0.061(5) 0.059(6) 0.061(6) -0.024(5) -0.020(5) 0.014(5) C43 0.058(5) 0.066(6) 0.064(6) -0.020(5) -0.029(5) 0.014(5) C44 0.056(5) 0.047(5) 0.058(5) -0.009(4) -0.015(4) 0.012(4) C45 0.070(6) 0.059(6) 0.071(6) -0.029(5) -0.027(5) 0.023(5) C46 0.065(6) 0.053(5) 0.058(6) -0.015(4) -0.029(5) 0.020(4) C47 0.080(7) 0.055(6) 0.107(9) -0.034(6) -0.024(6) 0.027(5) O5 0.047(4) 0.128(6) 0.067(4) -0.047(4) -0.018(3) 0.031(4) C51 0.040(4) 0.044(4) 0.040(5) -0.007(3) -0.009(4) -0.001(3) C52 0.048(5) 0.058(5) 0.043(5) -0.012(4) -0.014(4) 0.000(4) C56 0.046(5) 0.078(6) 0.046(5) -0.010(5) -0.015(4) 0.014(4) C53 0.043(5) 0.063(5) 0.052(5) -0.012(4) -0.020(4) 0.009(4) C55 0.058(6) 0.090(7) 0.040(5) -0.018(5) -0.015(4) 0.008(5) C54 0.036(4) 0.072(6) 0.056(6) -0.016(5) -0.008(4) 0.007(4) C57 0.053(6) 0.133(10) 0.071(7) -0.035(7) -0.006(5) 0.022(6) O6 0.095(5) 0.067(5) 0.126(7) -0.055(5) -0.020(5) -0.002(4) C61 0.037(4) 0.041(5) 0.060(6) -0.017(4) -0.012(4) 0.003(3) C62 0.069(6) 0.044(5) 0.085(7) -0.018(5) -0.005(5) -0.009(5) C63 0.068(6) 0.045(6) 0.121(10) -0.025(6) -0.016(7) -0.014(5) C64 0.068(6) 0.053(6) 0.098(9) -0.038(6) -0.013(6) -0.002(5) C65 0.092(7) 0.054(6) 0.089(8) -0.040(6) -0.022(6) 0.006(5) C66 0.077(6) 0.050(5) 0.075(7) -0.035(5) -0.012(5) -0.001(5) C67 0.118(10) 0.092(9) 0.133(12) -0.074(9) -0.038(9) 0.001(8) Cl1S 0.098(2) 0.106(2) 0.120(2) -0.0412(18) -0.0177(18) 0.0125(16) Cl2S 0.098(2) 0.106(2) 0.120(2) -0.0412(18) -0.0177(18) 0.0125(16) Cl3S 0.098(2) 0.106(2) 0.120(2) -0.0412(18) -0.0177(18) 0.0125(16) Cl4S 0.098(2) 0.106(2) 0.120(2) -0.0412(18) -0.0177(18) 0.0125(16) _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 Mo2 2.0902(9) . y Mo1 N3 2.109(6) . y Mo1 O8 2.124(5) . y Mo1 N5 2.145(6) . y Mo1 N1 2.156(6) . y Mo2 N4 2.122(6) . y Mo2 N2 2.129(6) . y Mo2 N6 2.136(6) . y Mo2 O7 2.162(5) . y N1 C1 1.323(9) . ? N1 C11 1.422(9) . ? N2 C1 1.324(9) . ? N2 C21 1.422(9) . ? N3 C2 1.333(10) . ? N3 C31 1.429(10) . ? N4 C2 1.321(10) . ? N4 C41 1.417(9) . ? N5 C3 1.323(10) . ? N5 C51 1.430(10) . ? N6 C3 1.315(10) . ? N6 C61 1.439(10) . ? O7 C4 1.262(8) . ? O8 C4 1.263(8) . ? C4 C5 1.489(10) . ? C5 C6 1.386(10) . ? C5 C7 1.401(10) 2_346 ? C6 F1 1.350(8) . ? C6 C7 1.353(10) . ? C7 F2 1.346(8) . ? C7 C5 1.401(10) 2_346 ? O1 C14 1.380(11) . ? O1 C17 1.399(14) . ? C11 C12 1.389(11) . ? C11 C16 1.396(11) . ? C12 C13 1.372(12) . ? C13 C14 1.382(13) . ? C14 C15 1.379(14) . ? C15 C16 1.374(12) . ? O2 C24 1.408(13) . ? O2 C27 1.424(17) . ? O2' C24 1.38(3) . ? O2' C27' 1.42(2) . ? C21 C26 1.372(11) . ? C21 C22 1.398(11) . ? C22 C23 1.371(12) . ? C23 C24 1.367(15) . ? C24 C25 1.398(16) . ? C25 C26 1.390(13) . ? O3 C34 1.395(10) . ? O3 C37 1.417(12) . ? C31 C36 1.374(11) . ? C31 C32 1.404(11) . ? C32 C33 1.360(12) . ? C33 C34 1.376(13) . ? C34 C35 1.347(12) . ? C35 C36 1.403(12) . ? O4 C44 1.367(10) . ? O4 C47 1.425(12) . ? C41 C42 1.383(11) . ? C41 C46 1.398(12) . ? C42 C43 1.387(12) . ? C43 C44 1.413(13) . ? C44 C45 1.372(12) . ? C45 C46 1.374(12) . ? O5 C54 1.353(10) . ? O5 C57 1.447(12) . ? C51 C56 1.395(12) . ? C51 C52 1.401(11) . ? C52 C53 1.374(11) . ? C56 C55 1.363(12) . ? C53 C54 1.381(12) . ? C55 C54 1.396(12) . ? O6 C64 1.382(11) . ? O6 C67 1.459(15) . ? C61 C62 1.364(12) . ? C61 C66 1.396(13) . ? C62 C63 1.412(14) . ? C63 C64 1.370(15) . ? C64 C65 1.327(14) . ? C65 C66 1.382(13) . ? C1S Cl1S 1.672(17) . ? C1S Cl2S 1.706(16) . ? C1S' Cl3S 1.68(3) . ? C1S' Cl4S 1.71(3) . ? C2S C3S 1.38(2) 1_565 ? C2S C5S 1.582(10) . ? C3S C2S 1.38(2) 1_545 ? C3S C4S 1.57(3) 2_245 ? C3S Cl6S 1.73(3) 2_245 ? C4S C4S 1.46(6) 2_155 ? C4S C3S 1.57(3) 2_245 ? Cl6S C3S 1.73(3) 2_245 ? 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 Mo2 Mo1 N3 93.36(16) . . y Mo2 Mo1 O8 93.14(12) . . y N3 Mo1 O8 173.3(2) . . y Mo2 Mo1 N5 91.61(17) . . y N3 Mo1 N5 92.7(2) . . y O8 Mo1 N5 85.4(2) . . y Mo2 Mo1 N1 91.34(15) . . y N3 Mo1 N1 94.6(2) . . y O8 Mo1 N1 86.9(2) . . y N5 Mo1 N1 171.9(2) . . y Mo1 Mo2 N4 91.97(16) . . y Mo1 Mo2 N2 93.76(16) . . y N4 Mo2 N2 93.1(2) . . y Mo1 Mo2 N6 93.30(17) . . y N4 Mo2 N6 94.1(2) . . y N2 Mo2 N6 169.7(2) . . y Mo1 Mo2 O7 90.44(12) . . y N4 Mo2 O7 177.4(2) . . y N2 Mo2 O7 87.7(2) . . y N6 Mo2 O7 84.8(2) . . y C1 N1 C11 116.3(6) . . ? C1 N1 Mo1 118.2(5) . . ? C11 N1 Mo1 125.3(5) . . ? C1 N2 C21 116.9(6) . . ? C1 N2 Mo2 117.1(5) . . ? C21 N2 Mo2 124.7(5) . . ? C2 N3 C31 120.1(6) . . ? C2 N3 Mo1 117.3(5) . . ? C31 N3 Mo1 121.4(5) . . ? C2 N4 C41 117.2(6) . . ? C2 N4 Mo2 118.2(5) . . ? C41 N4 Mo2 124.5(5) . . ? C3 N5 C51 118.2(6) . . ? C3 N5 Mo1 118.1(5) . . ? C51 N5 Mo1 121.7(5) . . ? C3 N6 C61 119.0(6) . . ? C3 N6 Mo2 117.3(5) . . ? C61 N6 Mo2 122.8(5) . . ? C4 O7 Mo2 116.6(4) . . ? C4 O8 Mo1 116.1(4) . . ? N1 C1 N2 119.1(7) . . ? N4 C2 N3 119.0(6) . . ? N6 C3 N5 119.1(7) . . ? O7 C4 O8 123.6(6) . . ? O7 C4 C5 119.2(6) . . ? O8 C4 C5 117.3(6) . . ? C6 C5 C7 115.0(6) . 2_346 ? C6 C5 C4 122.6(6) . . ? C7 C5 C4 122.4(7) 2_346 . ? F1 C6 C7 117.0(6) . . ? F1 C6 C5 120.0(6) . . ? C7 C6 C5 123.0(6) . . ? F2 C7 C6 118.2(6) . . ? F2 C7 C5 119.8(6) . 2_346 ? C6 C7 C5 122.0(6) . 2_346 ? C14 O1 C17 117.0(10) . . ? C12 C11 C16 117.6(7) . . ? C12 C11 N1 123.1(7) . . ? C16 C11 N1 119.2(7) . . ? C13 C12 C11 120.9(8) . . ? C12 C13 C14 120.4(9) . . ? C15 C14 O1 124.4(9) . . ? C15 C14 C13 119.8(8) . . ? O1 C14 C13 115.7(9) . . ? C16 C15 C14 119.5(8) . . ? C15 C16 C11 121.7(9) . . ? C24 O2 C27 112.3(13) . . ? C24 O2' C27' 112(3) . . ? C26 C21 C22 117.0(7) . . ? C26 C21 N2 122.6(7) . . ? C22 C21 N2 120.5(7) . . ? C23 C22 C21 122.3(9) . . ? C24 C23 C22 119.7(10) . . ? C23 C24 O2' 145.4(15) . . ? C23 C24 C25 119.9(8) . . ? O2' C24 C25 94.6(14) . . ? C23 C24 O2 110.3(11) . . ? O2' C24 O2 35.1(10) . . ? C25 C24 O2 129.7(11) . . ? C26 C25 C24 119.0(9) . . ? C21 C26 C25 122.1(9) . . ? C34 O3 C37 116.9(8) . . ? C36 C31 C32 117.4(7) . . ? C36 C31 N3 119.1(7) . . ? C32 C31 N3 123.3(7) . . ? C33 C32 C31 121.0(8) . . ? C32 C33 C34 120.6(8) . . ? C35 C34 C33 119.9(8) . . ? C35 C34 O3 124.2(8) . . ? C33 C34 O3 115.9(8) . . ? C34 C35 C36 120.1(8) . . ? C31 C36 C35 120.9(8) . . ? C44 O4 C47 116.0(7) . . ? C42 C41 C46 118.0(7) . . ? C42 C41 N4 122.8(7) . . ? C46 C41 N4 119.2(7) . . ? C41 C42 C43 120.9(8) . . ? C42 C43 C44 119.6(8) . . ? O4 C44 C45 125.6(8) . . ? O4 C44 C43 114.8(8) . . ? C45 C44 C43 119.6(8) . . ? C44 C45 C46 119.8(9) . . ? C45 C46 C41 122.0(8) . . ? C54 O5 C57 116.7(7) . . ? C56 C51 C52 117.5(7) . . ? C56 C51 N5 121.0(7) . . ? C52 C51 N5 121.5(7) . . ? C53 C52 C51 121.6(8) . . ? C55 C56 C51 121.4(8) . . ? C52 C53 C54 119.6(7) . . ? C56 C55 C54 120.2(8) . . ? O5 C54 C53 115.5(7) . . ? O5 C54 C55 124.9(8) . . ? C53 C54 C55 119.7(8) . . ? C64 O6 C67 114.3(9) . . ? C62 C61 C66 117.2(8) . . ? C62 C61 N6 123.8(8) . . ? C66 C61 N6 119.0(7) . . ? C61 C62 C63 120.1(10) . . ? C64 C63 C62 120.5(9) . . ? C65 C64 C63 119.8(9) . . ? C65 C64 O6 126.6(11) . . ? C63 C64 O6 113.5(9) . . ? C64 C65 C66 120.5(11) . . ? C65 C66 C61 121.8(9) . . ? Cl1S C1S Cl2S 115.4(10) . . ? Cl3S C1S' Cl4S 129(3) . . ? C3S C2S C5S 130.4(17) 1_565 . ? C2S C3S C4S 107.5(18) 1_545 2_245 ? C2S C3S Cl6S 135.2(17) 1_545 2_245 ? C4S C3S Cl6S 67.1(16) 2_245 2_245 ? C4S C4S C3S 113(3) 2_155 2_245 ? _diffrn_measured_fraction_theta_max 0.951 _diffrn_reflns_theta_full 22.53 _diffrn_measured_fraction_theta_full 0.951 _refine_diff_density_max 0.991 _refine_diff_density_min -0.958 _refine_diff_density_rms 0.119 #===END