# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Xiaoming Lu' _publ_contact_author_email lu-xiaoming@126.com loop_ _publ_author_name 'Xiaoming Lu' 'Xudong Shi' # Attachment '- compound2.cif' data_100201G _database_code_depnum_ccdc_archive 'CCDC 764951' _audit_creation_method SHELXL-97 _chemical_formula_moiety ; 4(C9 H14 Mo N2 O5), 4(C3 H12 N2), 2(C0.8 H2 O0.2) ; _chemical_formula_sum 'C24.80 H54 Mo2 N8 O10.20' _chemical_formula_weight 819.44 _chemical_melting_point ? _chemical_name_common ? _chemical_name_systematic ? 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' O O 0.0106 0.0060 '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' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_IT_number 2 _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 'x, y, z' 2 '-x, -y, -z' _cell_angle_alpha 100.168(2) _cell_angle_beta 91.3540(10) _cell_angle_gamma 90.0950(10) _cell_formula_units_Z 2 _cell_length_a 11.3739(10) _cell_length_b 12.4797(11) _cell_length_c 13.2237(15) _cell_measurement_reflns_used 3158 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 27.047 _cell_measurement_theta_min 2.432 _cell_volume 1847.0(3) _exptl_absorpt_coefficient_mu 0.737 _exptl_absorpt_correction_T_max 0.9103 _exptl_absorpt_correction_T_min 0.8146 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Bruker, 2000)' _exptl_crystal_F_000 849 _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.13 _exptl_special_details ? _diffrn_ambient_temperature 298(2) _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.961 _diffrn_measured_fraction_theta_max 0.961 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.1196 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 9119 _diffrn_reflns_theta_full 25.02 _diffrn_reflns_theta_max 25.02 _diffrn_reflns_theta_min 1.79 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _reflns_number_gt 3724 _reflns_number_total 6266 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'Bruker SMART' _computing_data_collection 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _computing_publication_material ; OLEX2: a complete structure solution, refinement and analysis program. Dolomanov et al., J. Appl. Cryst. (2009). 42, 339-341 ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _refine_diff_density_max 1.871 _refine_diff_density_min -1.672 _refine_diff_density_rms 0.197 _refine_ls_R_factor_all 0.1369 _refine_ls_R_factor_gt 0.0778 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 444 _refine_ls_number_reflns 6266 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.100 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_wR_factor_gt 0.1933 _refine_ls_wR_factor_ref 0.2501 _refine_ls_weighting_details ; calc w=1/[\s^2^(Fo^2^)+(0.1296P)^2^+3.9864P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _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. ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap 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 0.74801(8) 0.13618(7) 0.06650(7) 0.0309(3) Uani 1 1 d . . . Mo2 Mo 0.75266(8) 0.61176(7) 0.93274(7) 0.0282(3) Uani 1 1 d . . . N1 N 0.7462(9) -0.0247(7) 0.1402(8) 0.043(2) Uani 1 1 d . . . H1A H 0.7852 -0.0762 0.0978 0.051 Uiso 1 1 calc R . . H1B H 0.7884 -0.0105 0.1995 0.051 Uiso 1 1 calc R . . N2 N 0.4641(11) -0.2712(10) 0.1276(12) 0.074(4) Uani 1 1 d . . . H2B H 0.424(16) -0.223(15) 0.105(14) 0.088 Uiso 1 1 d . . . H2C H 0.518(17) -0.322(15) 0.105(15) 0.088 Uiso 1 1 d . . . N3 N 0.7521(9) 0.4246(7) 0.8568(8) 0.042(2) Uani 1 1 d . . . H3A H 0.7106 0.3888 0.8976 0.050 Uiso 1 1 calc R . . H3B H 0.7119 0.4181 0.7966 0.050 Uiso 1 1 calc R . . N4 N 1.0325(12) 0.1819(10) 0.8641(13) 0.084(4) Uani 1 1 d . . . H4B H 1.053(18) 0.246(17) 0.901(16) 0.101 Uiso 1 1 d . . . H4C H 0.984(18) 0.148(16) 0.901(16) 0.101 Uiso 1 1 d . . . N5 N 0.9051(8) 0.4294(7) 0.1360(7) 0.034(2) Uani 1 1 d . . . H5A H 0.8612 0.3711 0.1111 0.051 Uiso 1 1 calc R . . H5B H 0.9792 0.4090 0.1441 0.051 Uiso 1 1 calc R . . H5C H 0.9022 0.4761 0.0924 0.051 Uiso 1 1 calc R . . N6 N 0.5939(8) 0.4268(7) 0.1285(8) 0.039(2) Uani 1 1 d . . . H6A H 0.5991 0.4715 0.0833 0.059 Uiso 1 1 calc R . . H6B H 0.5194 0.4060 0.1318 0.059 Uiso 1 1 calc R . . H6C H 0.6384 0.3686 0.1088 0.059 Uiso 1 1 calc R . . N7 N 0.5961(8) 0.8779(7) 0.8666(8) 0.039(2) Uani 1 1 d . . . H7A H 0.6387 0.8278 0.8906 0.058 Uiso 1 1 calc R . . H7B H 0.5210 0.8571 0.8604 0.058 Uiso 1 1 calc R . . H7C H 0.6025 0.9411 0.9099 0.058 Uiso 1 1 calc R . . N8 N 0.9060(8) 0.8790(7) 0.8723(8) 0.039(2) Uani 1 1 d . . . H8A H 0.8975 0.9403 0.9173 0.059 Uiso 1 1 calc R . . H8B H 0.9816 0.8607 0.8696 0.059 Uiso 1 1 calc R . . H8C H 0.8644 0.8260 0.8917 0.059 Uiso 1 1 calc R . . O1 O 0.6375(7) 0.1792(6) 0.1935(6) 0.0385(19) Uani 1 1 d . . . O2 O 0.8633(7) 0.1749(6) 0.1958(6) 0.0405(19) Uani 1 1 d . . . O3 O 0.7501(7) 0.2719(6) 0.0446(6) 0.0367(18) Uani 1 1 d . . . O4 O 0.8675(7) 0.0764(6) 0.0021(7) 0.046(2) Uani 1 1 d . . . O5 O 0.6244(7) 0.0805(6) -0.0036(6) 0.042(2) Uani 1 1 d . . . O6 O 0.8641(6) 0.6079(6) 0.8053(5) 0.0324(17) Uani 1 1 d . . . O7 O 0.6369(6) 0.6038(6) 0.8028(6) 0.0359(18) Uani 1 1 d . . . O8 O 0.7515(6) 0.7558(6) 0.9563(6) 0.0353(18) Uani 1 1 d . . . O9 O 0.8745(7) 0.5817(6) 1.0049(6) 0.0398(19) Uani 1 1 d . . . O10 O 0.6324(7) 0.5750(6) 0.9987(6) 0.0397(19) Uani 1 1 d . . . O11 O 0.287(9) 0.031(7) 0.500(6) 0.12(3) Uani 0.20 1 d P . . C1 C 0.6912(11) 0.2087(9) 0.2850(9) 0.040(3) Uani 1 1 d . . . C2 C 0.8146(11) 0.2065(10) 0.2870(9) 0.042(3) Uani 1 1 d . . . C3 C 0.8742(13) 0.2364(11) 0.3779(10) 0.054(3) Uani 1 1 d . . . H3 H 0.9560 0.2355 0.3805 0.065 Uiso 1 1 calc R . . C4 C 0.8099(15) 0.2693(13) 0.4691(12) 0.068(4) Uani 1 1 d . . . H4 H 0.8500 0.2891 0.5318 0.082 Uiso 1 1 calc R . . C5 C 0.6969(15) 0.2719(13) 0.4656(12) 0.068(4) Uani 1 1 d . . . H5 H 0.6576 0.2973 0.5259 0.081 Uiso 1 1 calc R . . C6 C 0.6310(13) 0.2385(11) 0.3758(10) 0.057(4) Uani 1 1 d . . . H6 H 0.5492 0.2361 0.3765 0.069 Uiso 1 1 calc R . . C7 C 0.6366(11) -0.0715(10) 0.1619(11) 0.051(3) Uani 1 1 d . . . H7D H 0.5924 -0.0904 0.0975 0.061 Uiso 1 1 calc R . . H7E H 0.5927 -0.0153 0.2052 0.061 Uiso 1 1 calc R . . C8 C 0.6386(12) -0.1678(11) 0.2115(11) 0.054(3) Uani 1 1 d . . . H8D H 0.6733 -0.1473 0.2799 0.065 Uiso 1 1 calc R . . H8E H 0.6891 -0.2219 0.1729 0.065 Uiso 1 1 calc R . . C9 C 0.5194(13) -0.2193(12) 0.2203(13) 0.065(4) Uani 1 1 d . . . H9A H 0.5284 -0.2725 0.2652 0.078 Uiso 1 1 calc R . . H9B H 0.4673 -0.1631 0.2535 0.078 Uiso 1 1 calc R . . C10 C 0.8108(10) 0.5964(9) 0.7134(9) 0.037(3) Uani 1 1 d . . . C11 C 0.6874(10) 0.5956(9) 0.7133(8) 0.034(3) Uani 1 1 d . . . C12 C 0.6263(12) 0.5834(11) 0.6199(10) 0.051(3) Uani 1 1 d . . . H12 H 0.5445 0.5828 0.6179 0.061 Uiso 1 1 calc R . . C13 C 0.6898(14) 0.5717(13) 0.5276(11) 0.066(4) Uani 1 1 d . . . H13 H 0.6498 0.5615 0.4644 0.079 Uiso 1 1 calc R . . C14 C 0.8078(14) 0.5756(12) 0.5316(11) 0.065(4) Uani 1 1 d . . . H14 H 0.8484 0.5705 0.4708 0.078 Uiso 1 1 calc R . . C15 C 0.8701(12) 0.5869(11) 0.6228(10) 0.051(3) Uani 1 1 d . . . H15 H 0.9519 0.5881 0.6234 0.062 Uiso 1 1 calc R . . C16 C 0.8615(11) 0.3681(10) 0.8370(11) 0.051(3) Uani 1 1 d . . . H16A H 0.9034 0.3712 0.9022 0.061 Uiso 1 1 calc R . . H16B H 0.9082 0.4079 0.7954 0.061 Uiso 1 1 calc R . . C17 C 0.8565(12) 0.2531(10) 0.7854(11) 0.054(3) Uani 1 1 d . . . H17A H 0.8203 0.2496 0.7178 0.065 Uiso 1 1 calc R . . H17B H 0.8061 0.2133 0.8242 0.065 Uiso 1 1 calc R . . C18 C 0.9737(14) 0.1970(12) 0.7736(13) 0.067(4) Uani 1 1 d . . . H18A H 0.9620 0.1262 0.7306 0.080 Uiso 1 1 calc R . . H18B H 1.0247 0.2389 0.7373 0.080 Uiso 1 1 calc R . . C19 C 0.8605(11) 0.4813(9) 0.2348(9) 0.040(3) Uani 1 1 d . . . H19A H 0.9209 0.5299 0.2700 0.048 Uiso 1 1 calc R . . H19B H 0.8472 0.4254 0.2759 0.048 Uiso 1 1 calc R . . C20 C 0.7475(10) 0.5458(9) 0.2307(9) 0.039(3) Uani 1 1 d . . . H20A H 0.7476 0.6040 0.2899 0.047 Uiso 1 1 calc R . . H20B H 0.7485 0.5793 0.1699 0.047 Uiso 1 1 calc R . . C21 C 0.6342(11) 0.4825(10) 0.2286(9) 0.043(3) Uani 1 1 d . . . H21A H 0.6441 0.4291 0.2732 0.052 Uiso 1 1 calc R . . H21B H 0.5732 0.5323 0.2573 0.052 Uiso 1 1 calc R . . C22 C 0.6398(11) 0.8913(10) 0.7639(9) 0.044(3) Uani 1 1 d . . . H22A H 0.5789 0.9261 0.7287 0.053 Uiso 1 1 calc R . . H22B H 0.6527 0.8196 0.7236 0.053 Uiso 1 1 calc R . . C23 C 0.7517(12) 0.9569(10) 0.7667(10) 0.048(3) Uani 1 1 d . . . H23A H 0.7521 0.9906 0.7060 0.058 Uiso 1 1 calc R . . H23B H 0.7503 1.0149 0.8260 0.058 Uiso 1 1 calc R . . C24 C 0.8645(11) 0.8952(10) 0.7712(10) 0.044(3) Uani 1 1 d . . . H24A H 0.8545 0.8242 0.7280 0.053 Uiso 1 1 calc R . . H24B H 0.9255 0.9333 0.7414 0.053 Uiso 1 1 calc R . . C25 C 0.188(11) 0.102(10) 0.519(10) 0.12(4) Uani 0.20 1 d P . . H25A H 0.1947 0.1600 0.4791 0.141 Uiso 0.20 1 calc PR . . H25B H 0.1896 0.1356 0.5913 0.141 Uiso 0.20 1 calc PR . . C26 C 0.072(10) 0.042(9) 0.492(10) 0.12(4) Uani 0.20 1 d P . . H26A H 0.0537 0.0343 0.4201 0.177 Uiso 0.20 1 d PR . . H26B H 0.0110 0.0838 0.5303 0.177 Uiso 0.20 1 d PR . . H26C H 0.0759 -0.0284 0.5115 0.177 Uiso 0.20 1 d PR . . C27 C 0.399(12) 0.081(10) 0.522(10) 0.12(4) Uani 0.20 1 d P . . H27A H 0.4035 0.1152 0.5938 0.144 Uiso 0.20 1 calc PR . . H27B H 0.4083 0.1378 0.4811 0.144 Uiso 0.20 1 calc PR . . C28 C 0.5000 0.0000 0.5000 0.12(3) Uani 0.40 2 d SP . . H28A H 0.5693 0.0320 0.5360 0.178 Uiso 0.20 1 d PR . . H28B H 0.5149 -0.0178 0.4278 0.178 Uiso 0.20 1 d PR . . H28C H 0.4795 -0.0650 0.5252 0.178 Uiso 0.20 1 d PR . . 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 0.0280(6) 0.0263(5) 0.0381(6) 0.0049(4) 0.0010(4) 0.0001(4) Mo2 0.0264(6) 0.0284(5) 0.0313(6) 0.0093(4) 0.0006(4) 0.0013(4) N1 0.040(6) 0.035(5) 0.053(7) 0.008(4) 0.006(5) 0.004(4) N2 0.063(9) 0.062(8) 0.100(11) 0.019(7) 0.013(8) -0.012(6) N3 0.042(6) 0.035(5) 0.049(6) 0.010(4) 0.001(5) -0.003(4) N4 0.068(9) 0.064(8) 0.125(14) 0.030(8) 0.018(9) 0.021(7) N5 0.030(5) 0.036(5) 0.037(5) 0.011(4) -0.002(4) 0.002(4) N6 0.026(5) 0.043(6) 0.050(6) 0.014(5) -0.002(4) 0.001(4) N7 0.024(5) 0.038(5) 0.056(7) 0.013(4) -0.004(4) 0.001(4) N8 0.027(5) 0.036(5) 0.056(7) 0.009(4) 0.001(5) -0.002(4) O1 0.033(4) 0.041(4) 0.040(5) 0.002(3) -0.002(4) -0.002(3) O2 0.028(4) 0.048(5) 0.044(5) 0.008(4) -0.006(4) 0.001(3) O3 0.033(4) 0.030(4) 0.047(5) 0.006(3) 0.000(4) 0.002(3) O4 0.042(5) 0.048(5) 0.046(5) 0.005(4) 0.010(4) 0.004(4) O5 0.047(5) 0.037(4) 0.044(5) 0.009(4) 0.004(4) 0.000(4) O6 0.027(4) 0.045(4) 0.028(4) 0.012(3) 0.004(3) 0.002(3) O7 0.030(4) 0.049(5) 0.030(4) 0.010(3) -0.003(3) -0.001(3) O8 0.031(4) 0.033(4) 0.044(5) 0.011(3) 0.005(4) 0.004(3) O9 0.039(5) 0.039(4) 0.044(5) 0.016(4) 0.003(4) -0.001(4) O10 0.039(5) 0.042(5) 0.039(5) 0.011(3) 0.005(4) -0.002(4) O11 0.13(7) 0.12(6) 0.12(6) 0.02(5) 0.00(6) 0.00(5) C1 0.041(7) 0.041(7) 0.041(7) 0.012(5) 0.007(6) 0.000(5) C2 0.039(7) 0.047(7) 0.040(7) 0.009(5) 0.001(6) -0.005(5) C3 0.052(8) 0.065(9) 0.043(8) 0.006(6) 0.002(7) 0.000(7) C4 0.070(12) 0.081(11) 0.052(10) 0.005(8) -0.005(8) -0.005(9) C5 0.072(12) 0.085(11) 0.044(9) 0.001(7) 0.006(8) 0.001(9) C6 0.058(9) 0.069(9) 0.043(8) 0.005(7) 0.000(7) -0.001(7) C7 0.040(8) 0.051(8) 0.061(9) 0.009(6) 0.002(6) -0.003(6) C8 0.058(9) 0.050(8) 0.059(9) 0.018(6) 0.000(7) -0.003(6) C9 0.066(10) 0.057(9) 0.077(11) 0.023(8) 0.013(8) -0.005(8) C10 0.037(7) 0.045(7) 0.029(6) 0.007(5) 0.001(5) -0.002(5) C11 0.032(6) 0.042(6) 0.028(6) 0.007(5) 0.002(5) 0.004(5) C12 0.040(8) 0.071(9) 0.039(7) 0.006(6) -0.004(6) -0.002(6) C13 0.063(11) 0.091(11) 0.040(8) 0.006(7) -0.004(7) -0.009(8) C14 0.066(11) 0.086(11) 0.042(8) 0.010(7) 0.001(7) 0.004(8) C15 0.043(8) 0.071(9) 0.039(8) 0.006(6) 0.004(6) -0.004(6) C16 0.041(8) 0.050(8) 0.062(9) 0.010(6) 0.003(7) -0.007(6) C17 0.055(9) 0.048(8) 0.058(9) 0.004(6) 0.006(7) 0.002(6) C18 0.067(11) 0.058(9) 0.077(11) 0.015(8) 0.025(9) 0.016(8) C19 0.044(7) 0.045(7) 0.031(6) 0.006(5) -0.006(5) -0.004(5) C20 0.050(7) 0.039(6) 0.029(6) 0.006(5) 0.004(5) 0.004(5) C21 0.042(7) 0.046(7) 0.041(7) 0.008(5) 0.007(6) 0.008(6) C22 0.043(7) 0.050(7) 0.039(7) 0.006(5) -0.001(6) 0.005(6) C23 0.062(9) 0.044(7) 0.041(7) 0.016(6) 0.007(6) -0.005(6) C24 0.046(8) 0.046(7) 0.043(7) 0.016(6) 0.006(6) -0.002(6) C25 0.12(10) 0.12(9) 0.11(10) 0.02(7) 0.00(8) 0.01(8) C26 0.12(10) 0.12(9) 0.12(10) 0.02(7) 0.00(8) 0.01(7) C27 0.12(11) 0.12(10) 0.12(10) 0.02(7) 0.00(8) 0.00(8) C28 0.12(7) 0.12(6) 0.12(7) 0.02(5) 0.00(6) 0.01(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 Mo1 N1 2.382(9) . ? Mo1 O1 2.115(8) . ? Mo1 O2 2.116(8) . ? Mo1 O3 1.768(7) . ? Mo1 O4 1.722(8) . ? Mo1 O5 1.739(8) . ? Mo2 N3 2.374(9) . ? Mo2 O6 2.126(7) . ? Mo2 O7 2.127(7) . ? Mo2 O8 1.769(7) . ? Mo2 O9 1.743(8) . ? Mo2 O10 1.743(8) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N1 C7 1.432(15) . ? N2 H2B 0.89(18) . ? N2 H2C 0.89(19) . ? N2 C9 1.415(19) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N3 C16 1.438(15) . ? N4 H4B 0.9(2) . ? N4 H4C 0.9(2) . ? N4 C18 1.40(2) . ? N5 H5A 0.8900 . ? N5 H5B 0.8900 . ? N5 H5C 0.8900 . ? N5 C19 1.455(14) . ? N6 H6A 0.8900 . ? N6 H6B 0.8900 . ? N6 H6C 0.8900 . ? N6 C21 1.446(15) . ? N7 H7A 0.8900 . ? N7 H7B 0.8900 . ? N7 H7C 0.8900 . ? N7 C22 1.493(15) . ? N8 H8A 0.8900 . ? N8 H8B 0.8900 . ? N8 H8C 0.8900 . ? N8 C24 1.455(15) . ? O1 C1 1.333(14) . ? O2 C2 1.334(14) . ? O6 C10 1.330(13) . ? O7 C11 1.316(13) . ? O11 C25 1.43(12) . ? O11 C27 1.42(13) . ? C1 C2 1.404(17) . ? C1 C6 1.390(18) . ? C2 C3 1.359(17) . ? C3 H3 0.9300 . ? C3 C4 1.42(2) . ? C4 H4 0.9300 . ? C4 C5 1.29(2) . ? C5 H5 0.9300 . ? C5 C6 1.389(19) . ? C6 H6 0.9300 . ? C7 H7D 0.9700 . ? C7 H7E 0.9700 . ? C7 C8 1.467(18) . ? C8 H8D 0.9700 . ? C8 H8E 0.9700 . ? C8 C9 1.514(18) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.404(16) . ? C10 C15 1.377(17) . ? C11 C12 1.387(16) . ? C12 H12 0.9300 . ? C12 C13 1.419(19) . ? C13 H13 0.9300 . ? C13 C14 1.34(2) . ? C14 H14 0.9300 . ? C14 C15 1.369(19) . ? C15 H15 0.9300 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 C17 1.476(17) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C17 C18 1.505(19) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C19 C20 1.523(16) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C20 C21 1.507(17) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 C23 1.508(17) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C23 C24 1.502(17) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 C26 1.53(13) . ? C26 C26 2.0(2) 2_556 ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C27 C28 1.53(13) . ? C28 C27 1.53(13) 2_656 ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 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 Mo1 N1 H1A 107.3 . . ? Mo1 N1 H1B 107.3 . . ? Mo2 N3 H3A 107.3 . . ? Mo2 N3 H3B 107.3 . . ? N1 C7 H7D 107.7 . . ? N1 C7 H7E 107.7 . . ? N1 C7 C8 118.6(11) . . ? H1A N1 H1B 106.9 . . ? N2 C9 C8 116.7(13) . . ? N2 C9 H9A 108.1 . . ? N2 C9 H9B 108.1 . . ? H2B N2 H2C 139(19) . . ? N3 C16 H16A 107.8 . . ? N3 C16 H16B 107.8 . . ? N3 C16 C17 117.9(11) . . ? H3A N3 H3B 106.9 . . ? N4 C18 C17 116.7(13) . . ? N4 C18 H18A 108.1 . . ? N4 C18 H18B 108.1 . . ? H4B N4 H4C 109(10) . . ? N5 C19 H19A 108.3 . . ? N5 C19 H19B 108.3 . . ? N5 C19 C20 115.8(9) . . ? H5A N5 H5B 109.5 . . ? H5A N5 H5C 109.5 . . ? H5B N5 H5C 109.5 . . ? N6 C21 C20 115.7(10) . . ? N6 C21 H21A 108.4 . . ? N6 C21 H21B 108.4 . . ? H6A N6 H6B 109.5 . . ? H6A N6 H6C 109.5 . . ? H6B N6 H6C 109.5 . . ? N7 C22 H22A 108.5 . . ? N7 C22 H22B 108.5 . . ? N7 C22 C23 115.0(10) . . ? H7A N7 H7B 109.5 . . ? H7A N7 H7C 109.5 . . ? H7B N7 H7C 109.5 . . ? N8 C24 C23 116.8(11) . . ? N8 C24 H24A 108.1 . . ? N8 C24 H24B 108.1 . . ? H8A N8 H8B 109.5 . . ? H8A N8 H8C 109.5 . . ? H8B N8 H8C 109.5 . . ? O1 Mo1 N1 77.2(3) . . ? O1 Mo1 O2 74.7(3) . . ? O1 C1 C2 116.7(11) . . ? O1 C1 C6 123.3(12) . . ? O2 Mo1 N1 76.6(3) . . ? O2 C2 C1 115.1(11) . . ? O2 C2 C3 125.5(12) . . ? O3 Mo1 N1 165.5(4) . . ? O3 Mo1 O1 91.3(3) . . ? O3 Mo1 O2 92.0(3) . . ? O4 Mo1 N1 83.9(4) . . ? O4 Mo1 O1 155.8(4) . . ? O4 Mo1 O2 86.3(4) . . ? O4 Mo1 O3 104.5(4) . . ? O4 Mo1 O5 106.1(4) . . ? O5 Mo1 N1 85.3(4) . . ? O5 Mo1 O1 87.5(3) . . ? O5 Mo1 O2 156.9(4) . . ? O5 Mo1 O3 103.3(3) . . ? O6 Mo2 N3 77.1(3) . . ? O6 Mo2 O7 74.8(3) . . ? O6 C10 C11 115.8(10) . . ? O6 C10 C15 123.5(11) . . ? O7 Mo2 N3 76.2(3) . . ? O7 C11 C10 117.2(10) . . ? O7 C11 C12 124.1(11) . . ? O8 Mo2 N3 165.4(4) . . ? O8 Mo2 O6 91.6(3) . . ? O8 Mo2 O7 92.0(3) . . ? O9 Mo2 N3 86.2(3) . . ? O9 Mo2 O6 88.6(3) . . ? O9 Mo2 O7 158.0(3) . . ? O9 Mo2 O8 103.0(3) . . ? O9 Mo2 O10 104.4(4) . . ? O10 Mo2 N3 83.8(4) . . ? O10 Mo2 O6 156.2(3) . . ? O10 Mo2 O7 87.0(3) . . ? O10 Mo2 O8 104.5(3) . . ? O11 C25 H25A 109.2 . . ? O11 C25 H25B 109.2 . . ? O11 C25 C26 112(10) . . ? O11 C27 H27A 109.1 . . ? O11 C27 H27B 109.1 . . ? O11 C27 C28 113(9) . . ? C1 O1 Mo1 116.3(7) . . ? C1 C6 H6 121.1 . . ? C2 O2 Mo1 117.1(7) . . ? C2 C3 H3 120.4 . . ? C2 C3 C4 119.2(14) . . ? C3 C2 C1 119.4(12) . . ? C3 C4 H4 119.7 . . ? C4 C3 H3 120.4 . . ? C4 C5 H5 118.5 . . ? C4 C5 C6 123.0(15) . . ? C5 C4 C3 120.6(15) . . ? C5 C4 H4 119.7 . . ? C5 C6 C1 117.8(14) . . ? C5 C6 H6 121.1 . . ? C6 C1 C2 120.0(12) . . ? C6 C5 H5 118.5 . . ? C7 N1 Mo1 120.0(8) . . ? C7 N1 H1A 107.3 . . ? C7 N1 H1B 107.3 . . ? C7 C8 H8D 108.5 . . ? C7 C8 H8E 108.5 . . ? C7 C8 C9 114.9(12) . . ? H7D C7 H7E 107.1 . . ? C8 C7 H7D 107.7 . . ? C8 C7 H7E 107.7 . . ? C8 C9 H9A 108.1 . . ? C8 C9 H9B 108.1 . . ? H8D C8 H8E 107.5 . . ? C9 N2 H2B 109(10) . . ? C9 N2 H2C 109(10) . . ? C9 C8 H8D 108.5 . . ? C9 C8 H8E 108.5 . . ? H9A C9 H9B 107.3 . . ? C10 O6 Mo2 116.1(7) . . ? C10 C15 H15 120.3 . . ? C11 O7 Mo2 115.9(7) . . ? C11 C12 H12 120.3 . . ? C11 C12 C13 119.4(12) . . ? C12 C11 C10 118.7(11) . . ? C12 C13 H13 120.1 . . ? C13 C12 H12 120.3 . . ? C13 C14 H14 119.0 . . ? C13 C14 C15 121.9(15) . . ? C14 C13 C12 119.8(14) . . ? C14 C13 H13 120.1 . . ? C14 C15 C10 119.5(13) . . ? C14 C15 H15 120.3 . . ? C15 C10 C11 120.7(11) . . ? C15 C14 H14 119.0 . . ? C16 N3 Mo2 120.0(7) . . ? C16 N3 H3A 107.3 . . ? C16 N3 H3B 107.3 . . ? C16 C17 H17A 108.5 . . ? C16 C17 H17B 108.5 . . ? C16 C17 C18 114.9(12) . . ? H16A C16 H16B 107.2 . . ? C17 C16 H16A 107.8 . . ? C17 C16 H16B 107.8 . . ? C17 C18 H18A 108.1 . . ? C17 C18 H18B 108.1 . . ? H17A C17 H17B 107.5 . . ? C18 N4 H4B 109(10) . . ? C18 N4 H4C 109(10) . . ? C18 C17 H17A 108.5 . . ? C18 C17 H17B 108.5 . . ? H18A C18 H18B 107.3 . . ? C19 N5 H5A 109.5 . . ? C19 N5 H5B 109.5 . . ? C19 N5 H5C 109.5 . . ? C19 C20 H20A 108.2 . . ? C19 C20 H20B 108.2 . . ? H19A C19 H19B 107.4 . . ? C20 C19 H19A 108.3 . . ? C20 C19 H19B 108.3 . . ? C20 C21 H21A 108.4 . . ? C20 C21 H21B 108.4 . . ? H20A C20 H20B 107.4 . . ? C21 N6 H6A 109.5 . . ? C21 N6 H6B 109.5 . . ? C21 N6 H6C 109.5 . . ? C21 C20 C19 116.3(10) . . ? C21 C20 H20A 108.2 . . ? C21 C20 H20B 108.2 . . ? H21A C21 H21B 107.4 . . ? C22 N7 H7A 109.5 . . ? C22 N7 H7B 109.5 . . ? C22 N7 H7C 109.5 . . ? C22 C23 H23A 108.3 . . ? C22 C23 H23B 108.3 . . ? H22A C22 H22B 107.5 . . ? C23 C22 H22A 108.5 . . ? C23 C22 H22B 108.5 . . ? C23 C24 H24A 108.1 . . ? C23 C24 H24B 108.1 . . ? H23A C23 H23B 107.4 . . ? C24 N8 H8A 109.5 . . ? C24 N8 H8B 109.5 . . ? C24 N8 H8C 109.5 . . ? C24 C23 C22 116.1(10) . . ? C24 C23 H23A 108.3 . . ? C24 C23 H23B 108.3 . . ? H24A C24 H24B 107.3 . . ? C25 C26 C26 160(10) . 2_556 ? C25 C26 H26A 110.7 . . ? C25 C26 H26B 108.1 . . ? C25 C26 H26C 109.6 . . ? H25A C25 H25B 107.9 . . ? C26 C25 H25A 109.2 . . ? C26 C25 H25B 109.2 . . ? C26 C26 H26A 89.1 2_556 . ? C26 C26 H26B 65.9 2_556 . ? C26 C26 H26C 58.6 2_556 . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C27 O11 C25 116(9) . . ? C27 C28 C27 180(10) . 2_656 ? C27 C28 H28A 71.8 2_656 . ? C27 C28 H28A 108.2 . . ? C27 C28 H28B 111.7 . . ? C27 C28 H28B 68.3 2_656 . ? C27 C28 H28C 108.5 . . ? C27 C28 H28C 71.5 2_656 . ? H27A C27 H27B 107.8 . . ? C28 C27 H27A 109.1 . . ? C28 C27 H27B 109.1 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? 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 Mo1 N1 C7 C8 -177.3(10) . . . . ? Mo1 O1 C1 C2 -0.9(13) . . . . ? Mo1 O1 C1 C6 -179.5(10) . . . . ? Mo1 O2 C2 C1 0.7(13) . . . . ? Mo1 O2 C2 C3 -178.7(10) . . . . ? Mo2 N3 C16 C17 -177.3(10) . . . . ? Mo2 O6 C10 C11 4.1(12) . . . . ? Mo2 O6 C10 C15 -176.6(10) . . . . ? Mo2 O7 C11 C10 -1.8(13) . . . . ? Mo2 O7 C11 C12 176.3(9) . . . . ? N1 Mo1 O1 C1 80.3(8) . . . . ? N1 Mo1 O2 C2 -81.0(8) . . . . ? N1 C7 C8 C9 -173.2(12) . . . . ? N3 Mo2 O6 C10 75.2(7) . . . . ? N3 Mo2 O7 C11 -77.2(8) . . . . ? N3 C16 C17 C18 -176.1(13) . . . . ? N5 C19 C20 C21 87.1(13) . . . . ? N7 C22 C23 C24 85.7(13) . . . . ? O1 Mo1 N1 C7 51.2(9) . . . . ? O1 Mo1 O2 C2 -0.9(8) . . . . ? O1 C1 C2 O2 0.1(16) . . . . ? O1 C1 C2 C3 179.5(11) . . . . ? O1 C1 C6 C5 -177.4(12) . . . . ? O2 Mo1 N1 C7 128.3(10) . . . . ? O2 Mo1 O1 C1 0.9(7) . . . . ? O2 C2 C3 C4 179.4(12) . . . . ? O3 Mo1 N1 C7 89.7(16) . . . . ? O3 Mo1 O1 C1 -90.8(8) . . . . ? O3 Mo1 O2 C2 90.0(8) . . . . ? O4 Mo1 N1 C7 -144.1(10) . . . . ? O4 Mo1 O1 C1 40.7(12) . . . . ? O4 Mo1 O2 C2 -165.6(8) . . . . ? O5 Mo1 N1 C7 -37.3(10) . . . . ? O5 Mo1 O1 C1 166.0(8) . . . . ? O5 Mo1 O2 C2 -41.8(12) . . . . ? O6 Mo2 N3 C16 52.9(9) . . . . ? O6 Mo2 O7 C11 3.0(7) . . . . ? O6 C10 C11 O7 -1.5(15) . . . . ? O6 C10 C11 C12 -179.7(10) . . . . ? O6 C10 C15 C14 -179.8(12) . . . . ? O7 Mo2 N3 C16 130.1(10) . . . . ? O7 Mo2 O6 C10 -3.8(7) . . . . ? O7 C11 C12 C13 -177.9(12) . . . . ? O8 Mo2 N3 C16 92.9(16) . . . . ? O8 Mo2 O6 C10 -95.4(7) . . . . ? O8 Mo2 O7 C11 94.1(8) . . . . ? O9 Mo2 N3 C16 -36.5(10) . . . . ? O9 Mo2 O6 C10 161.6(7) . . . . ? O9 Mo2 O7 C11 -39.3(12) . . . . ? O10 Mo2 N3 C16 -141.5(10) . . . . ? O10 Mo2 O6 C10 37.6(12) . . . . ? O10 Mo2 O7 C11 -161.5(8) . . . . ? O11 C25 C26 C26 89(35) . . . 2_556 ? O11 C27 C28 C27 161(56) . . . 2_656 ? C1 C2 C3 C4 0(2) . . . . ? C2 C1 C6 C5 4.0(19) . . . . ? C2 C3 C4 C5 -1(2) . . . . ? C3 C4 C5 C6 3(3) . . . . ? C4 C5 C6 C1 -5(2) . . . . ? C6 C1 C2 O2 178.8(11) . . . . ? C6 C1 C2 C3 -1.8(18) . . . . ? C7 C8 C9 N2 68.8(18) . . . . ? C10 C11 C12 C13 0.2(19) . . . . ? C11 C10 C15 C14 -1(2) . . . . ? C11 C12 C13 C14 -2(2) . . . . ? C12 C13 C14 C15 2(2) . . . . ? C13 C14 C15 C10 -1(2) . . . . ? C15 C10 C11 O7 179.2(11) . . . . ? C15 C10 C11 C12 1.0(18) . . . . ? C16 C17 C18 N4 66.1(19) . . . . ? C19 C20 C21 N6 -84.2(13) . . . . ? C22 C23 C24 N8 -84.0(14) . . . . ? C25 O11 C27 C28 180(9) . . . . ? C27 O11 C25 C26 180(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1A N4 0.90 2.55 3.189(17) 128.9 2_756 N1 H1A O8 0.90 2.57 3.328(12) 141.8 1_544 N2 H2C O10 0.90(19) 2.2(2) 3.044(16) 159.2 1_544 N3 H3A N2 0.90 2.45 3.147(16) 134.7 2_656 N4 H4C O4 0.9(2) 2.2(2) 3.096(17) 175.0 1_556 N5 H5A O3 0.89 1.86 2.735(12) 167.0 . N5 H5B O6 0.89 1.92 2.783(11) 164.9 2_766 N5 H5C O9 0.89 1.92 2.807(12) 172.0 1_554 N6 H6A O10 0.89 1.89 2.777(12) 171.7 1_554 N6 H6B O7 0.89 2.01 2.845(12) 156.1 2_666 N6 H6B O10 0.89 2.44 3.039(12) 124.5 2_666 N6 H6C O3 0.89 1.87 2.733(12) 164.0 . N7 H7A O8 0.89 1.86 2.721(12) 165.0 . N7 H7B O1 0.89 1.95 2.809(12) 163.3 2_666 N7 H7B O5 0.89 2.56 3.119(12) 121.9 2_666 N7 H7C O5 0.89 1.92 2.807(12) 176.2 1_566 N8 H8A O4 0.89 1.90 2.784(13) 173.6 1_566 N8 H8B O2 0.89 2.00 2.838(12) 156.4 2_766 N8 H8B O4 0.89 2.41 3.029(13) 126.0 2_766 N8 H8C O8 0.89 1.87 2.715(12) 161.0 . data_sh1 _database_code_depnum_ccdc_archive 'CCDC 774454' #TrackingRef '- compound1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C8 H13 Mo N2 O5, 0.5(C2 H10 N2)' _chemical_formula_sum 'C9 H18 Mo N3 O5' _chemical_formula_weight 344.20 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _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 17.2729(12) _cell_length_b 6.4159(5) _cell_length_c 11.6210(9) _cell_angle_alpha 90.00 _cell_angle_beta 96.4500(10) _cell_angle_gamma 90.00 _cell_volume 1279.70(17) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 392 _cell_measurement_theta_min 3.16 _cell_measurement_theta_max 26.39 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.787 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 700 _exptl_absorpt_coefficient_mu 1.043 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6512 _exptl_absorpt_correction_T_max 0.6685 _exptl_absorpt_process_details '(SADABS; Sheldrick, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9417 _diffrn_reflns_av_R_equivalents 0.0210 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.19 _diffrn_reflns_theta_max 25.50 _reflns_number_total 2367 _reflns_number_gt 2231 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0663P)^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 2367 _refine_ls_number_parameters 165 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0200 _refine_ls_R_factor_gt 0.0173 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.163052(8) 0.33049(2) 0.222422(12) 0.01799(11) Uani 1 1 d . . . N1 N 0.22081(11) 0.1255(3) 0.07638(15) 0.0285(4) Uani 1 1 d . . . H1A H 0.1833 0.1015 0.0177 0.034 Uiso 1 1 calc R . . H1B H 0.2571 0.2053 0.0481 0.034 Uiso 1 1 calc R . . N2 N 0.21413(12) -0.3181(2) -0.05266(17) 0.0294(4) Uani 1 1 d . . . H2A H 0.1862 -0.3805 -0.0028 0.044 Uiso 1 1 calc R . . H2B H 0.2315 -0.4130 -0.0994 0.044 Uiso 1 1 calc R . . H2C H 0.1845 -0.2259 -0.0945 0.044 Uiso 1 1 calc R . . N3 N 0.02101(10) 0.8030(3) 0.12122(16) 0.0275(4) Uani 1 1 d . . . H3A H 0.0481 0.8936 0.1677 0.041 Uiso 1 1 calc R . . H3B H 0.0463 0.6820 0.1229 0.041 Uiso 1 1 calc R . . H3C H -0.0257 0.7839 0.1451 0.041 Uiso 1 1 calc R . . O1 O 0.25082(9) 0.16851(17) 0.33028(13) 0.0243(3) Uani 1 1 d . . . O2 O 0.26454(8) 0.4888(2) 0.20612(13) 0.0298(3) Uani 1 1 d . . . O3 O 0.11962(8) 0.4597(2) 0.09620(11) 0.0259(3) Uani 1 1 d . . . O4 O 0.13328(9) 0.4885(2) 0.33267(13) 0.0324(3) Uani 1 1 d . . . O5 O 0.10529(8) 0.1077(2) 0.23584(12) 0.0288(3) Uani 1 1 d . . . C1 C 0.32342(11) 0.2475(3) 0.33624(16) 0.0249(4) Uani 1 1 d . . . C2 C 0.33048(10) 0.4261(3) 0.26732(16) 0.0254(4) Uani 1 1 d . . . C3 C 0.40193(13) 0.5225(4) 0.2677(2) 0.0398(5) Uani 1 1 d . . . H3 H 0.4070 0.6390 0.2216 0.048 Uiso 1 1 calc R . . C4 C 0.46640(14) 0.4449(5) 0.3375(2) 0.0508(6) Uani 1 1 d . . . H4 H 0.5146 0.5098 0.3377 0.061 Uiso 1 1 calc R . . C5 C 0.45911(14) 0.2740(5) 0.4055(3) 0.0545(7) Uani 1 1 d . . . H5 H 0.5023 0.2244 0.4526 0.065 Uiso 1 1 calc R . . C6 C 0.38771(15) 0.1735(3) 0.4049(3) 0.0422(6) Uani 1 1 d . . . H6 H 0.3834 0.0564 0.4509 0.051 Uiso 1 1 calc R . . C7 C 0.25713(14) -0.0752(3) 0.11007(17) 0.0342(5) Uani 1 1 d . . . H7A H 0.2209 -0.1549 0.1507 0.041 Uiso 1 1 calc R . . H7B H 0.3029 -0.0487 0.1644 0.041 Uiso 1 1 calc R . . C8 C 0.28140(13) -0.2092(3) 0.01206(18) 0.0301(5) Uani 1 1 d . . . H8A H 0.3063 -0.1216 -0.0410 0.036 Uiso 1 1 calc R . . H8B H 0.3192 -0.3117 0.0438 0.036 Uiso 1 1 calc R . . C9 C 0.01153(12) 0.8853(3) 0.00122(17) 0.0282(4) Uani 1 1 d . . . H9A H -0.0282 0.8056 -0.0452 0.034 Uiso 1 1 calc R . . H9B H 0.0601 0.8691 -0.0324 0.034 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 0.02198(15) 0.01510(15) 0.01703(15) -0.00025(5) 0.00286(9) -0.00061(5) N1 0.0440(10) 0.0191(7) 0.0229(8) 0.0007(7) 0.0066(7) 0.0052(7) N2 0.0455(11) 0.0162(9) 0.0284(10) -0.0002(6) 0.0119(8) 0.0067(6) N3 0.0275(9) 0.0254(8) 0.0298(10) -0.0017(7) 0.0046(7) 0.0000(6) O1 0.0280(8) 0.0213(8) 0.0233(8) 0.0048(5) 0.0013(6) -0.0022(5) O2 0.0270(7) 0.0236(7) 0.0384(8) 0.0089(6) 0.0022(6) -0.0034(5) O3 0.0299(7) 0.0212(6) 0.0263(7) 0.0034(5) 0.0017(5) 0.0038(5) O4 0.0357(8) 0.0324(8) 0.0296(8) -0.0115(6) 0.0063(6) 0.0006(6) O5 0.0328(8) 0.0244(7) 0.0282(7) 0.0024(6) -0.0015(6) -0.0091(6) C1 0.0252(9) 0.0264(11) 0.0233(9) -0.0017(8) 0.0043(7) -0.0007(8) C2 0.0268(10) 0.0233(11) 0.0266(10) 0.0000(7) 0.0058(8) -0.0008(7) C3 0.0325(11) 0.0393(12) 0.0478(14) 0.0073(10) 0.0053(10) -0.0073(9) C4 0.0275(12) 0.0626(17) 0.0614(17) 0.0050(14) 0.0017(11) -0.0140(11) C5 0.0287(12) 0.0690(17) 0.0622(18) 0.0118(16) -0.0105(11) 0.0013(12) C6 0.0341(14) 0.0447(15) 0.0464(16) 0.0160(10) -0.0015(11) 0.0019(8) C7 0.0549(13) 0.0241(10) 0.0229(10) -0.0025(8) 0.0015(9) 0.0137(9) C8 0.0438(12) 0.0215(8) 0.0262(11) 0.0002(8) 0.0089(9) 0.0080(9) C9 0.0350(11) 0.0226(11) 0.0262(10) -0.0031(8) 0.0001(8) 0.0033(9) _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 O4 1.7554(13) . ? Mo1 O5 1.7600(14) . ? Mo1 O3 1.7760(13) . ? Mo1 O2 2.0532(14) . ? Mo1 O1 2.1266(14) . ? Mo1 N1 2.4466(17) . ? N1 C7 1.466(3) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C8 1.486(3) . ? N2 H2A 0.8900 . ? N2 H2B 0.8900 . ? N2 H2C 0.8900 . ? N3 C9 1.483(3) . ? N3 H3A 0.8900 . ? N3 H3B 0.8900 . ? N3 H3C 0.8900 . ? O1 C1 1.347(2) . ? O2 C2 1.335(2) . ? C1 C6 1.377(3) . ? C1 C2 1.411(3) . ? C2 C3 1.380(3) . ? C3 C4 1.394(4) . ? C3 H3 0.9300 . ? C4 C5 1.366(4) . ? C4 H4 0.9300 . ? C5 C6 1.391(4) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.523(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C9 1.524(4) 3_575 ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? 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 O4 Mo1 O5 100.88(7) . . ? O4 Mo1 O3 101.66(7) . . ? O5 Mo1 O3 105.14(6) . . ? O4 Mo1 O2 96.02(6) . . ? O5 Mo1 O2 155.28(6) . . ? O3 Mo1 O2 88.78(6) . . ? O4 Mo1 O1 95.74(6) . . ? O5 Mo1 O1 85.68(6) . . ? O3 Mo1 O1 157.20(6) . . ? O2 Mo1 O1 74.73(5) . . ? O4 Mo1 N1 172.95(7) . . ? O5 Mo1 N1 84.51(6) . . ? O3 Mo1 N1 81.10(6) . . ? O2 Mo1 N1 77.47(6) . . ? O1 Mo1 N1 80.03(6) . . ? C7 N1 Mo1 118.85(12) . . ? C7 N1 H1A 107.6 . . ? Mo1 N1 H1A 107.6 . . ? C7 N1 H1B 107.6 . . ? Mo1 N1 H1B 107.6 . . ? H1A N1 H1B 107.0 . . ? C8 N2 H2A 109.5 . . ? C8 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C8 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C9 N3 H3A 109.5 . . ? C9 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? C9 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? C1 O1 Mo1 116.38(11) . . ? C2 O2 Mo1 119.19(12) . . ? O1 C1 C6 125.84(19) . . ? O1 C1 C2 114.56(16) . . ? C6 C1 C2 119.56(18) . . ? O2 C2 C3 125.1(2) . . ? O2 C2 C1 115.10(16) . . ? C3 C2 C1 119.76(18) . . ? C2 C3 C4 119.8(2) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 120.3(2) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C4 C5 C6 120.6(2) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 120.0(2) . . ? C1 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? N1 C7 C8 116.19(16) . . ? N1 C7 H7A 108.2 . . ? C8 C7 H7A 108.2 . . ? N1 C7 H7B 108.2 . . ? C8 C7 H7B 108.2 . . ? H7A C7 H7B 107.4 . . ? N2 C8 C7 112.25(18) . . ? N2 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? N2 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? N3 C9 C9 111.3(2) . 3_575 ? N3 C9 H9A 109.4 . . ? C9 C9 H9A 109.4 3_575 . ? N3 C9 H9B 109.4 . . ? C9 C9 H9B 109.4 3_575 . ? H9A C9 H9B 108.0 . . ? 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 N1 C7 -58.09(16) . . . . ? O3 Mo1 N1 C7 -164.39(17) . . . . ? O2 Mo1 N1 C7 104.89(17) . . . . ? O1 Mo1 N1 C7 28.47(16) . . . . ? O4 Mo1 O1 C1 -93.09(13) . . . . ? O5 Mo1 O1 C1 166.38(13) . . . . ? O3 Mo1 O1 C1 46.6(2) . . . . ? O2 Mo1 O1 C1 1.60(13) . . . . ? N1 Mo1 O1 C1 81.21(13) . . . . ? O4 Mo1 O2 C2 92.41(15) . . . . ? O5 Mo1 O2 C2 -40.7(2) . . . . ? O3 Mo1 O2 C2 -166.00(14) . . . . ? O1 Mo1 O2 C2 -1.92(14) . . . . ? N1 Mo1 O2 C2 -84.84(14) . . . . ? Mo1 O1 C1 C6 176.58(19) . . . . ? Mo1 O1 C1 C2 -1.1(2) . . . . ? Mo1 O2 C2 C3 -177.55(17) . . . . ? Mo1 O2 C2 C1 2.0(2) . . . . ? O1 C1 C2 O2 -0.5(3) . . . . ? C6 C1 C2 O2 -178.3(2) . . . . ? O1 C1 C2 C3 179.06(18) . . . . ? C6 C1 C2 C3 1.2(3) . . . . ? O2 C2 C3 C4 178.5(2) . . . . ? C1 C2 C3 C4 -1.0(3) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C3 C4 C5 C6 0.9(5) . . . . ? O1 C1 C6 C5 -178.0(2) . . . . ? C2 C1 C6 C5 -0.4(4) . . . . ? C4 C5 C6 C1 -0.7(5) . . . . ? Mo1 N1 C7 C8 171.46(15) . . . . ? N1 C7 C8 N2 -77.8(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3C O5 0.89 2.35 3.147(2) 149.4 2 N3 H3C O4 0.89 2.31 3.021(2) 136.4 2 N3 H3B O3 0.89 1.95 2.819(2) 163.3 . N3 H3A O5 0.89 1.82 2.698(2) 168.4 1_565 N2 H2C O4 0.89 1.91 2.789(2) 168.8 4_565 N2 H2B O1 0.89 1.88 2.739(2) 162.0 4 N2 H2A O3 0.89 2.00 2.885(2) 174.3 1_545 N1 H1B O1 0.90 2.65 3.245(2) 124.6 4_565 N1 H1A O4 0.90 2.30 3.143(2) 156.2 4_565 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.409 _refine_diff_density_min -0.345 _refine_diff_density_rms 0.135