# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Nadia Carmen Moesch-Zanetti' _publ_contact_author_email NADIA.MOESCH@UNI-GRAZ.AT _publ_section_title ; Oxo-Molybdenum and Oxo-Tungsten Complexes of Schiff Bases Relevant to Molybdoenzymes ; loop_ _publ_author_name 'Nadia Carmen Moesch-Zanetti' 'Judith Baumgartner' 'Ferdinand Belaj' 'Regine Herbst-Irmer' ; V.Jancik ; 'Martina Judmaier' 'Ganna Lyashenko' 'Gerald Saischek' # Attachment 'structure1.cif' data_456j _database_code_depnum_ccdc_archive 'CCDC 695364' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H96 Mo2 N4 O8' _chemical_formula_weight 1289.37 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' 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 monoclinic _symmetry_space_group_name_H-M Pc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' _cell_length_a 11.691(2) _cell_length_b 16.641(3) _cell_length_c 16.834(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.48(3) _cell_angle_gamma 90.00 _cell_volume 3220.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7450 _cell_measurement_theta_min 4.885 _cell_measurement_theta_max 52.355 _exptl_crystal_description blocks _exptl_crystal_colour orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.446 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8280 _exptl_absorpt_correction_T_max 0.9083 _exptl_absorpt_process_details SADABS _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 'SMART APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25106 _diffrn_reflns_av_R_equivalents 0.0563 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 26.36 _reflns_number_total 6561 _reflns_number_gt 6172 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0994P)^2^+2.7023P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.27(13) _refine_ls_number_reflns 6561 _refine_ls_number_parameters 740 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0679 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1576 _refine_ls_wR_factor_gt 0.1542 _refine_ls_goodness_of_fit_ref 1.130 _refine_ls_restrained_S_all 1.130 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 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 0.58678(4) 0.01164(4) 0.53194(4) 0.0106(2) Uani 1 1 d . . . Mo2 Mo 0.57923(4) 0.48797(4) 0.01745(4) 0.0113(2) Uani 1 1 d . . . N1 N 0.3981(9) 0.0142(4) 0.4937(6) 0.013(2) Uani 1 1 d . . . N2 N 0.7735(9) 0.0096(5) 0.5484(6) 0.012(2) Uani 1 1 d . . . N3 N 0.3904(9) 0.4855(4) 0.0099(6) 0.012(2) Uani 1 1 d . . . N4 N 0.7657(9) 0.4899(5) 0.0511(6) 0.015(2) Uani 1 1 d . . . O1 O 0.5774(5) 0.1106(4) 0.5594(4) 0.0225(15) Uani 1 1 d . . . O2 O 0.5991(5) -0.0396(5) 0.6204(4) 0.0223(14) Uani 1 1 d . . . O3 O 0.6056(5) 0.0502(4) 0.4151(4) 0.0173(13) Uani 1 1 d . . . O4 O 0.5644(5) -0.0941(4) 0.4662(4) 0.0191(13) Uani 1 1 d . . . O5 O 0.5912(5) 0.5375(5) -0.0682(4) 0.0236(15) Uani 1 1 d . . . O6 O 0.5701(5) 0.3886(4) -0.0118(4) 0.0207(15) Uani 1 1 d . . . O7 O 0.5955(5) 0.4511(4) 0.1404(4) 0.0149(12) Uani 1 1 d . . . O8 O 0.5587(5) 0.5943(4) 0.0778(4) 0.0192(13) Uani 1 1 d . . . C1 C 0.6522(7) 0.1372(5) 0.3137(5) 0.0203(17) Uani 1 1 d . . . H1A H 0.5718 0.1245 0.2887 0.030 Uiso 1 1 calc R . . H1B H 0.7050 0.1194 0.2782 0.030 Uiso 1 1 calc R . . H1C H 0.6600 0.1954 0.3221 0.030 Uiso 1 1 calc R . . C2 C 0.6825(6) 0.0946(4) 0.3943(5) 0.0129(15) Uani 1 1 d . . . C3 C 0.7933(7) 0.1030(4) 0.4400(5) 0.0148(15) Uani 1 1 d . . . H3A H 0.8424 0.1428 0.4235 0.018 Uiso 1 1 calc R . . C4 C 0.8388(7) 0.0571(5) 0.5091(5) 0.0131(15) Uani 1 1 d . . . C5 C 0.9685(7) 0.0647(5) 0.5388(5) 0.0224(18) Uani 1 1 d . . . H5A H 0.9918 0.0301 0.5861 0.034 Uiso 1 1 calc R . . H5B H 0.9877 0.1206 0.5537 0.034 Uiso 1 1 calc R . . H5C H 1.0100 0.0482 0.4959 0.034 Uiso 1 1 calc R . . C6 C 0.8362(6) -0.0396(5) 0.6136(5) 0.0140(15) Uani 1 1 d . . . C7 C 0.8638(7) -0.1178(5) 0.5971(5) 0.0165(16) Uani 1 1 d . . . C8 C 0.9184(7) -0.1652(5) 0.6617(5) 0.0202(17) Uani 1 1 d . . . H8A H 0.9398 -0.2189 0.6520 0.024 Uiso 1 1 calc R . . C9 C 0.9415(7) -0.1348(5) 0.7391(5) 0.0211(18) Uani 1 1 d . . . H9A H 0.9757 -0.1685 0.7825 0.025 Uiso 1 1 calc R . . C10 C 0.9158(8) -0.0569(5) 0.7543(5) 0.0220(18) Uani 1 1 d . . . H10A H 0.9349 -0.0367 0.8078 0.026 Uiso 1 1 calc R . . C11 C 0.8608(8) -0.0055(5) 0.6909(6) 0.017(2) Uani 1 1 d . . . C12 C 0.8353(7) 0.0799(5) 0.7114(5) 0.0189(17) Uani 1 1 d . . . H12A H 0.8048 0.1084 0.6596 0.023 Uiso 1 1 calc R . . C13 C 0.9455(8) 0.1239(6) 0.7525(6) 0.023(2) Uani 1 1 d . . . H13A H 1.0045 0.1211 0.7180 0.034 Uiso 1 1 calc R . . H13B H 0.9756 0.0985 0.8046 0.034 Uiso 1 1 calc R . . H13C H 0.9269 0.1803 0.7611 0.034 Uiso 1 1 calc R . . C14 C 0.7415(7) 0.0849(6) 0.7647(5) 0.0252(19) Uani 1 1 d . . . H14A H 0.6709 0.0574 0.7377 0.038 Uiso 1 1 calc R . . H14B H 0.7237 0.1414 0.7735 0.038 Uiso 1 1 calc R . . H14C H 0.7703 0.0590 0.8169 0.038 Uiso 1 1 calc R . . C15 C 0.8381(7) -0.1527(5) 0.5128(5) 0.0181(16) Uani 1 1 d . . . H15A H 0.7853 -0.1147 0.4776 0.022 Uiso 1 1 calc R . . C16 C 0.7773(8) -0.2335(5) 0.5106(6) 0.028(2) Uani 1 1 d . . . H16A H 0.7051 -0.2276 0.5318 0.041 Uiso 1 1 calc R . . H16B H 0.8284 -0.2721 0.5438 0.041 Uiso 1 1 calc R . . H16C H 0.7593 -0.2529 0.4547 0.041 Uiso 1 1 calc R . . C17 C 0.9506(8) -0.1602(7) 0.4787(6) 0.032(2) Uani 1 1 d . . . H17A H 0.9889 -0.1077 0.4804 0.049 Uiso 1 1 calc R . . H17B H 0.9321 -0.1790 0.4226 0.049 Uiso 1 1 calc R . . H17C H 1.0027 -0.1988 0.5111 0.049 Uiso 1 1 calc R . . C18 C 0.5162(7) -0.1975(5) 0.3689(6) 0.0241(19) Uani 1 1 d . . . H18A H 0.5993 -0.2089 0.3859 0.036 Uiso 1 1 calc R . . H18B H 0.4997 -0.1869 0.3107 0.036 Uiso 1 1 calc R . . H18C H 0.4707 -0.2439 0.3810 0.036 Uiso 1 1 calc R . . C19 C 0.4844(7) -0.1254(5) 0.4132(5) 0.0182(16) Uani 1 1 d . . . C20 C 0.3729(6) -0.0972(4) 0.3990(4) 0.0124(14) Uani 1 1 d . . . H20A H 0.3189 -0.1234 0.3582 0.015 Uiso 1 1 calc R . . C21 C 0.3312(7) -0.0327(5) 0.4394(5) 0.0143(15) Uani 1 1 d . . . C22 C 0.2021(7) -0.0162(5) 0.4167(6) 0.0235(19) Uani 1 1 d . . . H22A H 0.1819 0.0298 0.4478 0.035 Uiso 1 1 calc R . . H22B H 0.1586 -0.0636 0.4287 0.035 Uiso 1 1 calc R . . H22C H 0.1823 -0.0041 0.3589 0.035 Uiso 1 1 calc R . . C23 C 0.3394(6) 0.0749(5) 0.5335(5) 0.0142(16) Uani 1 1 d . . . C24 C 0.3174(7) 0.1507(5) 0.4996(5) 0.0210(18) Uani 1 1 d . . . C25 C 0.2617(7) 0.2076(5) 0.5398(5) 0.0194(16) Uani 1 1 d . . . H25A H 0.2462 0.2597 0.5172 0.023 Uiso 1 1 calc R . . C26 C 0.2293(7) 0.1889(5) 0.6118(6) 0.0255(19) Uani 1 1 d . . . H26A H 0.1906 0.2280 0.6384 0.031 Uiso 1 1 calc R . . C27 C 0.2520(7) 0.1145(6) 0.6459(6) 0.0198(19) Uani 1 1 d . . . H27A H 0.2307 0.1034 0.6966 0.024 Uiso 1 1 calc R . . C28 C 0.3058(6) 0.0546(5) 0.6076(5) 0.0143(16) Uani 1 1 d . . . C29 C 0.3230(7) -0.0296(6) 0.6430(6) 0.0170(18) Uani 1 1 d . . . H29A H 0.3712 -0.0610 0.6105 0.020 Uiso 1 1 calc R . . C30 C 0.3882(8) -0.0264(6) 0.7306(6) 0.029(2) Uani 1 1 d . . . H30A H 0.4620 0.0021 0.7328 0.043 Uiso 1 1 calc R . . H30B H 0.4036 -0.0812 0.7510 0.043 Uiso 1 1 calc R . . H30C H 0.3406 0.0019 0.7639 0.043 Uiso 1 1 calc R . . C31 C 0.2070(8) -0.0742(6) 0.6404(6) 0.029(2) Uani 1 1 d . . . H31A H 0.1642 -0.0758 0.5847 0.044 Uiso 1 1 calc R . . H31B H 0.1605 -0.0460 0.6746 0.044 Uiso 1 1 calc R . . H31C H 0.2225 -0.1292 0.6604 0.044 Uiso 1 1 calc R . . C32 C 0.3542(7) 0.1754(5) 0.4199(5) 0.0196(17) Uani 1 1 d . . . H32A H 0.3944 0.1285 0.3998 0.023 Uiso 1 1 calc R . . C33 C 0.2481(9) 0.1963(6) 0.3560(6) 0.032(2) Uani 1 1 d . . . H33A H 0.1940 0.1508 0.3488 0.048 Uiso 1 1 calc R . . H33B H 0.2730 0.2081 0.3047 0.048 Uiso 1 1 calc R . . H33C H 0.2092 0.2436 0.3735 0.048 Uiso 1 1 calc R . . C34 C 0.4395(9) 0.2473(5) 0.4307(6) 0.028(2) Uani 1 1 d . . . H34A H 0.5075 0.2342 0.4719 0.042 Uiso 1 1 calc R . . H34B H 0.4005 0.2947 0.4478 0.042 Uiso 1 1 calc R . . H34C H 0.4644 0.2586 0.3794 0.042 Uiso 1 1 calc R . . C35 C 0.6407(7) 0.3634(5) 0.2534(5) 0.0207(17) Uani 1 1 d . . . H35A H 0.5599 0.3760 0.2571 0.031 Uiso 1 1 calc R . . H35B H 0.6924 0.3817 0.3026 0.031 Uiso 1 1 calc R . . H35C H 0.6491 0.3052 0.2476 0.031 Uiso 1 1 calc R . . C36 C 0.6724(7) 0.4055(4) 0.1810(5) 0.0136(15) Uani 1 1 d . . . C37 C 0.7824(6) 0.3971(4) 0.1635(5) 0.0120(14) Uani 1 1 d . . . H37A H 0.8315 0.3576 0.1929 0.014 Uiso 1 1 calc R . . C38 C 0.8281(7) 0.4419(5) 0.1062(5) 0.0150(16) Uani 1 1 d . . . C39 C 0.9572(7) 0.4324(5) 0.1100(5) 0.0213(17) Uani 1 1 d . . . H39A H 0.9820 0.4660 0.0685 0.032 Uiso 1 1 calc R . . H39B H 0.9750 0.3760 0.1008 0.032 Uiso 1 1 calc R . . H39C H 0.9985 0.4491 0.1634 0.032 Uiso 1 1 calc R . . C40 C 0.8288(6) 0.5390(5) 0.0015(5) 0.0160(16) Uani 1 1 d . . . C41 C 0.8609(6) 0.6171(5) 0.0263(5) 0.0147(15) Uani 1 1 d . . . C42 C 0.9133(7) 0.6651(5) -0.0241(6) 0.0224(18) Uani 1 1 d . . . H42A H 0.9347 0.7187 -0.0086 0.027 Uiso 1 1 calc R . . C43 C 0.9349(7) 0.6355(5) -0.0975(5) 0.0213(18) Uani 1 1 d . . . H43A H 0.9706 0.6690 -0.1317 0.026 Uiso 1 1 calc R . . C44 C 0.9047(7) 0.5580(5) -0.1204(5) 0.0205(17) Uani 1 1 d . . . H44A H 0.9207 0.5386 -0.1703 0.025 Uiso 1 1 calc R . . C45 C 0.8510(7) 0.5067(5) -0.0724(6) 0.018(2) Uani 1 1 d . . . C46 C 0.8258(7) 0.4210(5) -0.0988(5) 0.0170(16) Uani 1 1 d . . . H46A H 0.7942 0.3923 -0.0552 0.020 Uiso 1 1 calc R . . C47 C 0.7329(7) 0.4176(5) -0.1776(5) 0.0262(19) Uani 1 1 d . . . H47A H 0.6622 0.4453 -0.1689 0.039 Uiso 1 1 calc R . . H47B H 0.7145 0.3614 -0.1920 0.039 Uiso 1 1 calc R . . H47C H 0.7633 0.4439 -0.2214 0.039 Uiso 1 1 calc R . . C48 C 0.9368(8) 0.3774(6) -0.1119(6) 0.027(2) Uani 1 1 d . . . H48A H 0.9951 0.3797 -0.0622 0.041 Uiso 1 1 calc R . . H48B H 0.9675 0.4036 -0.1558 0.041 Uiso 1 1 calc R . . H48C H 0.9185 0.3212 -0.1262 0.041 Uiso 1 1 calc R . . C49 C 0.8414(7) 0.6504(5) 0.1062(5) 0.0193(17) Uani 1 1 d . . . H49A H 0.7919 0.6113 0.1300 0.023 Uiso 1 1 calc R . . C50 C 0.9579(8) 0.6588(7) 0.1652(6) 0.035(2) Uani 1 1 d . . . H50A H 0.9978 0.6067 0.1709 0.052 Uiso 1 1 calc R . . H50B H 0.9434 0.6764 0.2180 0.052 Uiso 1 1 calc R . . H50C H 1.0067 0.6985 0.1442 0.052 Uiso 1 1 calc R . . C51 C 0.7788(8) 0.7305(5) 0.0969(6) 0.0260(19) Uani 1 1 d . . . H51A H 0.7046 0.7246 0.0595 0.039 Uiso 1 1 calc R . . H51B H 0.8271 0.7703 0.0756 0.039 Uiso 1 1 calc R . . H51C H 0.7643 0.7483 0.1497 0.039 Uiso 1 1 calc R . . C52 C 0.5113(7) 0.6974(5) 0.1624(6) 0.0261(19) Uani 1 1 d . . . H52A H 0.5945 0.7084 0.1663 0.039 Uiso 1 1 calc R . . H52B H 0.4947 0.6869 0.2165 0.039 Uiso 1 1 calc R . . H52C H 0.4662 0.7440 0.1389 0.039 Uiso 1 1 calc R . . C53 C 0.4787(7) 0.6256(5) 0.1101(5) 0.0180(16) Uani 1 1 d . . . C54 C 0.3666(7) 0.5977(4) 0.0965(5) 0.0144(15) Uani 1 1 d . . . H54A H 0.3126 0.6242 0.1234 0.017 Uiso 1 1 calc R . . C55 C 0.3252(6) 0.5325(5) 0.0453(5) 0.0119(15) Uani 1 1 d . . . C56 C 0.1959(8) 0.5185(6) 0.0341(6) 0.029(2) Uani 1 1 d . . . H56A H 0.1747 0.4724 -0.0018 0.043 Uiso 1 1 calc R . . H56B H 0.1546 0.5664 0.0102 0.043 Uiso 1 1 calc R . . H56C H 0.1743 0.5076 0.0866 0.043 Uiso 1 1 calc R . . C57 C 0.3316(7) 0.4236(5) -0.0448(5) 0.0156(16) Uani 1 1 d . . . C58 C 0.2947(6) 0.4437(5) -0.1267(5) 0.0191(17) Uani 1 1 d . . . C59 C 0.2383(7) 0.3826(6) -0.1769(5) 0.0187(19) Uani 1 1 d . . . H59A H 0.2127 0.3938 -0.2326 0.022 Uiso 1 1 calc R . . C60 C 0.2190(7) 0.3086(6) -0.1490(6) 0.026(2) Uani 1 1 d . . . H60A H 0.1811 0.2688 -0.1848 0.031 Uiso 1 1 calc R . . C61 C 0.2550(7) 0.2912(5) -0.0677(5) 0.0204(17) Uani 1 1 d . . . H61A H 0.2395 0.2395 -0.0483 0.024 Uiso 1 1 calc R . . C62 C 0.3136(6) 0.3478(5) -0.0134(5) 0.0219(18) Uani 1 1 d . . . C63 C 0.3512(7) 0.3247(5) 0.0732(5) 0.0181(16) Uani 1 1 d . . . H63A H 0.3940 0.3714 0.1021 0.022 Uiso 1 1 calc R . . C64 C 0.2482(8) 0.3058(7) 0.1140(6) 0.033(2) Uani 1 1 d . . . H64A H 0.1950 0.3518 0.1083 0.049 Uiso 1 1 calc R . . H64B H 0.2762 0.2950 0.1715 0.049 Uiso 1 1 calc R . . H64C H 0.2071 0.2584 0.0886 0.049 Uiso 1 1 calc R . . C65 C 0.4342(8) 0.2515(5) 0.0837(6) 0.0263(19) Uani 1 1 d . . . H65A H 0.5016 0.2631 0.0584 0.040 Uiso 1 1 calc R . . H65B H 0.3931 0.2043 0.0580 0.040 Uiso 1 1 calc R . . H65C H 0.4606 0.2409 0.1414 0.040 Uiso 1 1 calc R . . C66 C 0.3107(8) 0.5259(5) -0.1606(5) 0.0141(18) Uani 1 1 d . . . H66A H 0.3574 0.5587 -0.1165 0.017 Uiso 1 1 calc R . . C67 C 0.1946(9) 0.5681(6) -0.1869(7) 0.038(2) Uani 1 1 d . . . H67A H 0.1525 0.5696 -0.1416 0.056 Uiso 1 1 calc R . . H67B H 0.1484 0.5388 -0.2321 0.056 Uiso 1 1 calc R . . H67C H 0.2082 0.6231 -0.2039 0.056 Uiso 1 1 calc R . . C68 C 0.3775(8) 0.5222(6) -0.2296(6) 0.033(2) Uani 1 1 d . . . H68A H 0.4522 0.4952 -0.2114 0.050 Uiso 1 1 calc R . . H68B H 0.3914 0.5768 -0.2474 0.050 Uiso 1 1 calc R . . H68C H 0.3322 0.4921 -0.2747 0.050 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 0.0094(4) 0.0129(3) 0.0097(5) -0.0007(4) 0.0018(3) 0.0011(4) Mo2 0.0084(4) 0.0153(4) 0.0101(5) -0.0004(4) 0.0017(3) -0.0011(4) N1 0.013(5) 0.005(4) 0.021(5) -0.003(3) 0.002(4) -0.003(3) N2 0.013(5) 0.022(5) 0.002(4) 0.001(3) 0.000(3) 0.000(3) N3 0.011(4) 0.008(4) 0.018(5) 0.001(3) 0.002(4) 0.000(3) N4 0.012(5) 0.028(5) 0.005(4) 0.003(3) 0.003(4) 0.005(3) O1 0.004(3) 0.031(4) 0.031(4) -0.012(3) -0.001(2) -0.001(2) O2 0.014(3) 0.035(4) 0.017(3) 0.007(3) 0.002(2) 0.002(3) O3 0.008(3) 0.023(3) 0.020(3) 0.003(3) 0.002(2) 0.002(2) O4 0.008(3) 0.012(3) 0.036(3) -0.008(2) 0.001(2) 0.001(2) O5 0.010(3) 0.032(4) 0.028(4) 0.007(3) 0.003(2) -0.002(3) O6 0.008(3) 0.026(4) 0.028(4) -0.013(3) 0.005(3) -0.001(2) O7 0.012(3) 0.016(3) 0.017(3) 0.004(2) 0.002(2) -0.006(2) O8 0.004(3) 0.022(3) 0.031(3) -0.006(3) 0.001(2) 0.003(2) C1 0.022(4) 0.020(4) 0.018(4) 0.007(3) 0.003(3) -0.002(3) C2 0.011(4) 0.008(3) 0.022(4) -0.002(3) 0.009(3) 0.004(3) C3 0.019(4) 0.011(4) 0.016(4) 0.000(3) 0.009(3) -0.001(3) C4 0.014(4) 0.015(4) 0.012(3) -0.001(3) 0.006(3) 0.008(3) C5 0.016(4) 0.029(5) 0.025(4) 0.002(3) 0.010(3) 0.001(3) C6 0.001(3) 0.026(4) 0.015(4) 0.008(3) 0.003(3) 0.001(3) C7 0.014(4) 0.020(4) 0.017(4) 0.010(3) 0.007(3) -0.001(3) C8 0.021(4) 0.017(4) 0.025(4) 0.009(3) 0.008(3) 0.000(3) C9 0.016(4) 0.029(5) 0.019(4) 0.011(3) 0.005(3) 0.001(3) C10 0.023(4) 0.029(5) 0.016(4) 0.001(3) 0.007(3) 0.004(4) C11 0.013(4) 0.027(5) 0.012(5) 0.014(3) 0.003(3) -0.003(3) C12 0.019(4) 0.027(4) 0.011(4) -0.001(3) 0.005(3) -0.002(3) C13 0.020(4) 0.032(5) 0.016(5) -0.005(4) 0.002(3) -0.003(4) C14 0.018(4) 0.035(5) 0.024(5) -0.013(4) 0.010(3) -0.001(4) C15 0.021(4) 0.008(4) 0.026(4) -0.003(3) 0.007(3) 0.004(3) C16 0.035(5) 0.018(5) 0.032(5) 0.005(3) 0.009(4) 0.000(4) C17 0.020(4) 0.053(6) 0.027(5) -0.007(4) 0.010(4) -0.002(4) C18 0.019(4) 0.020(4) 0.034(5) -0.019(4) 0.007(3) 0.001(3) C19 0.024(4) 0.019(4) 0.014(4) -0.005(3) 0.008(3) -0.001(3) C20 0.014(4) 0.015(4) 0.008(3) -0.001(3) 0.002(3) -0.003(3) C21 0.015(4) 0.015(4) 0.013(4) 0.002(3) 0.004(3) 0.001(3) C22 0.020(4) 0.025(5) 0.024(5) -0.006(3) 0.002(3) -0.001(3) C23 0.004(3) 0.017(4) 0.023(4) -0.009(3) 0.003(3) 0.001(3) C24 0.010(4) 0.026(4) 0.025(4) -0.010(3) -0.002(3) -0.005(3) C25 0.017(4) 0.016(4) 0.026(4) 0.000(3) 0.008(3) -0.001(3) C26 0.016(4) 0.024(4) 0.036(5) -0.008(4) 0.006(4) 0.002(3) C27 0.013(4) 0.030(5) 0.019(4) -0.013(4) 0.009(3) -0.005(3) C28 0.005(3) 0.025(5) 0.011(4) -0.005(3) -0.001(3) 0.003(3) C29 0.010(4) 0.030(5) 0.012(4) -0.008(4) 0.005(3) 0.003(4) C30 0.021(5) 0.042(6) 0.021(5) 0.001(4) -0.002(3) -0.002(4) C31 0.013(4) 0.034(5) 0.038(5) 0.009(4) -0.003(4) -0.006(4) C32 0.021(4) 0.019(4) 0.018(4) -0.003(3) 0.003(3) 0.002(3) C33 0.039(6) 0.030(5) 0.022(5) 0.004(4) -0.007(4) 0.006(4) C34 0.036(6) 0.016(4) 0.031(5) -0.003(3) 0.003(4) -0.001(4) C35 0.022(4) 0.018(4) 0.021(4) 0.010(3) 0.004(3) 0.005(3) C36 0.020(4) 0.005(3) 0.015(4) 0.002(3) 0.000(3) -0.006(3) C37 0.013(4) 0.004(3) 0.018(4) 0.004(3) -0.001(3) 0.001(3) C38 0.013(4) 0.015(4) 0.016(4) -0.005(3) 0.003(3) -0.007(3) C39 0.013(4) 0.030(5) 0.022(4) 0.005(3) 0.005(3) 0.006(3) C40 0.006(3) 0.029(5) 0.014(4) 0.011(3) 0.004(3) -0.003(3) C41 0.014(4) 0.014(4) 0.017(4) 0.007(3) 0.004(3) -0.003(3) C42 0.011(4) 0.025(5) 0.032(5) 0.006(4) 0.007(3) -0.004(3) C43 0.023(4) 0.015(4) 0.027(5) 0.013(3) 0.009(3) 0.002(3) C44 0.014(4) 0.036(5) 0.014(4) 0.006(3) 0.007(3) 0.002(4) C45 0.007(4) 0.027(5) 0.019(5) 0.008(3) 0.004(3) 0.004(3) C46 0.023(4) 0.026(4) 0.004(4) -0.001(3) 0.007(3) 0.002(3) C47 0.023(5) 0.031(5) 0.023(4) -0.008(4) -0.002(3) -0.003(4) C48 0.029(5) 0.030(5) 0.028(5) 0.002(4) 0.016(4) 0.004(4) C49 0.020(4) 0.020(4) 0.018(4) 0.002(3) 0.003(3) -0.009(3) C50 0.027(5) 0.049(6) 0.024(5) -0.003(4) -0.005(4) 0.003(4) C51 0.029(5) 0.023(5) 0.026(5) -0.001(3) 0.006(4) -0.004(4) C52 0.021(4) 0.024(5) 0.032(5) -0.010(4) 0.003(4) 0.004(3) C53 0.025(4) 0.013(4) 0.015(4) 0.003(3) 0.003(3) 0.005(3) C54 0.018(4) 0.012(4) 0.015(4) -0.003(3) 0.007(3) 0.003(3) C55 0.008(4) 0.011(4) 0.017(4) 0.006(3) 0.000(3) 0.002(3) C56 0.014(4) 0.034(5) 0.040(6) -0.011(4) 0.012(4) -0.001(4) C57 0.010(4) 0.018(4) 0.018(4) -0.010(3) 0.001(3) 0.000(3) C58 0.005(3) 0.035(5) 0.019(4) -0.006(4) 0.006(3) 0.001(3) C59 0.008(4) 0.033(5) 0.013(4) -0.003(4) -0.004(3) 0.002(3) C60 0.014(4) 0.032(5) 0.031(5) -0.022(4) 0.003(3) 0.000(3) C61 0.015(4) 0.018(4) 0.029(5) -0.003(3) 0.004(3) -0.003(3) C62 0.003(3) 0.031(5) 0.032(5) -0.007(4) 0.004(3) -0.001(3) C63 0.015(4) 0.012(4) 0.029(4) -0.005(3) 0.009(3) -0.004(3) C64 0.026(5) 0.044(6) 0.032(5) 0.002(4) 0.016(4) -0.005(4) C65 0.028(5) 0.023(4) 0.029(5) 0.000(4) 0.008(4) -0.001(4) C66 0.020(4) 0.020(4) 0.002(4) 0.004(3) 0.001(3) 0.004(3) C67 0.033(6) 0.039(6) 0.046(6) 0.010(5) 0.021(5) 0.016(5) C68 0.023(5) 0.048(6) 0.032(5) 0.004(4) 0.013(4) 0.006(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 O2 1.699(7) . ? Mo1 O1 1.720(7) . ? Mo1 O4 2.070(6) . ? Mo1 O3 2.119(6) . ? Mo1 N2 2.150(11) . ? Mo1 N1 2.183(10) . ? Mo2 O5 1.688(7) . ? Mo2 O6 1.723(6) . ? Mo2 O8 2.076(6) . ? Mo2 O7 2.135(6) . ? Mo2 N4 2.151(11) . ? Mo2 N3 2.188(10) . ? N1 C21 1.340(12) . ? N1 C23 1.452(11) . ? N2 C4 1.352(13) . ? N2 C6 1.456(12) . ? N3 C55 1.309(12) . ? N3 C57 1.466(12) . ? N4 C38 1.336(13) . ? N4 C40 1.460(13) . ? O3 C2 1.261(9) . ? O4 C19 1.281(10) . ? O7 C36 1.275(9) . ? O8 C53 1.276(10) . ? C1 C2 1.515(10) . ? C2 C3 1.388(11) . ? C3 C4 1.413(10) . ? C4 C5 1.513(11) . ? C6 C7 1.380(12) . ? C6 C11 1.401(13) . ? C7 C8 1.400(11) . ? C7 C15 1.512(11) . ? C8 C9 1.378(12) . ? C9 C10 1.365(12) . ? C10 C11 1.426(12) . ? C11 C12 1.505(12) . ? C12 C13 1.534(11) . ? C12 C14 1.541(11) . ? C15 C16 1.518(11) . ? C15 C17 1.533(11) . ? C18 C19 1.495(10) . ? C19 C20 1.365(11) . ? C20 C21 1.405(11) . ? C21 C22 1.513(11) . ? C23 C24 1.389(12) . ? C23 C28 1.414(11) . ? C24 C25 1.393(11) . ? C24 C32 1.538(12) . ? C25 C26 1.369(13) . ? C26 C27 1.371(13) . ? C27 C28 1.398(11) . ? C28 C29 1.522(12) . ? C29 C30 1.532(12) . ? C29 C31 1.539(12) . ? C32 C33 1.527(11) . ? C32 C34 1.548(12) . ? C35 C36 1.511(11) . ? C36 C37 1.377(11) . ? C37 C38 1.400(10) . ? C38 C39 1.506(11) . ? C40 C41 1.395(11) . ? C40 C45 1.422(13) . ? C41 C42 1.387(11) . ? C41 C49 1.510(11) . ? C42 C43 1.395(13) . ? C43 C44 1.375(12) . ? C44 C45 1.399(12) . ? C45 C46 1.507(12) . ? C46 C48 1.537(12) . ? C46 C47 1.555(11) . ? C49 C51 1.514(12) . ? C49 C50 1.539(12) . ? C52 C53 1.492(11) . ? C53 C54 1.369(11) . ? C54 C55 1.416(11) . ? C55 C56 1.507(11) . ? C57 C62 1.399(12) . ? C57 C58 1.408(11) . ? C58 C59 1.408(12) . ? C58 C66 1.507(12) . ? C59 C60 1.350(13) . ? C60 C61 1.388(13) . ? C61 C62 1.401(11) . ? C62 C63 1.495(12) . ? C63 C64 1.524(11) . ? C63 C65 1.547(12) . ? C66 C68 1.516(12) . ? C66 C67 1.520(13) . ? 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 O1 104.2(4) . . ? O2 Mo1 O4 91.3(3) . . ? O1 Mo1 O4 161.8(3) . . ? O2 Mo1 O3 163.6(3) . . ? O1 Mo1 O3 89.0(3) . . ? O4 Mo1 O3 77.6(3) . . ? O2 Mo1 N2 87.5(3) . . ? O1 Mo1 N2 95.3(3) . . ? O4 Mo1 N2 94.7(3) . . ? O3 Mo1 N2 81.4(3) . . ? O2 Mo1 N1 100.9(3) . . ? O1 Mo1 N1 87.2(3) . . ? O4 Mo1 N1 80.6(3) . . ? O3 Mo1 N1 89.4(3) . . ? N2 Mo1 N1 170.4(5) . . ? O5 Mo2 O6 103.6(4) . . ? O5 Mo2 O8 92.1(3) . . ? O6 Mo2 O8 162.0(3) . . ? O5 Mo2 O7 164.2(3) . . ? O6 Mo2 O7 89.5(3) . . ? O8 Mo2 O7 76.6(3) . . ? O5 Mo2 N4 88.9(3) . . ? O6 Mo2 N4 95.6(3) . . ? O8 Mo2 N4 93.5(3) . . ? O7 Mo2 N4 80.9(3) . . ? O5 Mo2 N3 101.5(3) . . ? O6 Mo2 N3 87.5(3) . . ? O8 Mo2 N3 80.7(3) . . ? O7 Mo2 N3 87.8(3) . . ? N4 Mo2 N3 168.3(5) . . ? C21 N1 C23 117.0(9) . . ? C21 N1 Mo1 128.5(7) . . ? C23 N1 Mo1 114.5(6) . . ? C4 N2 C6 116.4(9) . . ? C4 N2 Mo1 125.3(7) . . ? C6 N2 Mo1 117.8(7) . . ? C55 N3 C57 117.3(9) . . ? C55 N3 Mo2 128.9(7) . . ? C57 N3 Mo2 113.7(6) . . ? C38 N4 C40 117.5(9) . . ? C38 N4 Mo2 125.0(7) . . ? C40 N4 Mo2 116.8(6) . . ? C2 O3 Mo1 129.3(5) . . ? C19 O4 Mo1 136.3(5) . . ? C36 O7 Mo2 128.3(5) . . ? C53 O8 Mo2 135.7(5) . . ? O3 C2 C3 123.2(7) . . ? O3 C2 C1 117.3(7) . . ? C3 C2 C1 119.4(7) . . ? C2 C3 C4 125.1(7) . . ? N2 C4 C3 123.9(8) . . ? N2 C4 C5 120.5(8) . . ? C3 C4 C5 115.6(7) . . ? C7 C6 C11 123.5(7) . . ? C7 C6 N2 118.9(7) . . ? C11 C6 N2 117.5(8) . . ? C6 C7 C8 117.7(8) . . ? C6 C7 C15 122.5(7) . . ? C8 C7 C15 119.8(7) . . ? C9 C8 C7 120.7(8) . . ? C10 C9 C8 121.0(8) . . ? C9 C10 C11 120.9(8) . . ? C6 C11 C10 116.1(8) . . ? C6 C11 C12 125.4(8) . . ? C10 C11 C12 118.4(8) . . ? C11 C12 C13 111.7(7) . . ? C11 C12 C14 112.1(7) . . ? C13 C12 C14 109.9(7) . . ? C7 C15 C16 112.0(7) . . ? C7 C15 C17 110.3(7) . . ? C16 C15 C17 110.3(7) . . ? O4 C19 C20 122.4(7) . . ? O4 C19 C18 117.2(7) . . ? C20 C19 C18 120.3(7) . . ? C19 C20 C21 125.6(7) . . ? N1 C21 C20 124.4(8) . . ? N1 C21 C22 119.9(8) . . ? C20 C21 C22 115.7(7) . . ? C24 C23 C28 121.2(7) . . ? C24 C23 N1 120.6(8) . . ? C28 C23 N1 118.2(8) . . ? C23 C24 C25 119.1(8) . . ? C23 C24 C32 122.7(7) . . ? C25 C24 C32 118.2(8) . . ? C26 C25 C24 120.3(8) . . ? C25 C26 C27 120.8(8) . . ? C26 C27 C28 121.3(8) . . ? C27 C28 C23 117.2(8) . . ? C27 C28 C29 121.0(7) . . ? C23 C28 C29 121.8(7) . . ? C28 C29 C30 110.6(7) . . ? C28 C29 C31 112.3(7) . . ? C30 C29 C31 109.0(8) . . ? C33 C32 C24 110.8(7) . . ? C33 C32 C34 109.2(7) . . ? C24 C32 C34 112.4(7) . . ? O7 C36 C37 122.7(7) . . ? O7 C36 C35 117.1(7) . . ? C37 C36 C35 120.1(7) . . ? C36 C37 C38 125.6(7) . . ? N4 C38 C37 124.6(8) . . ? N4 C38 C39 120.6(8) . . ? C37 C38 C39 114.8(7) . . ? C41 C40 C45 122.2(7) . . ? C41 C40 N4 119.1(8) . . ? C45 C40 N4 118.7(8) . . ? C42 C41 C40 118.5(8) . . ? C42 C41 C49 119.3(7) . . ? C40 C41 C49 122.2(7) . . ? C41 C42 C43 120.7(8) . . ? C44 C43 C42 120.0(8) . . ? C43 C44 C45 122.1(8) . . ? C44 C45 C40 116.5(8) . . ? C44 C45 C46 119.5(8) . . ? C40 C45 C46 124.0(8) . . ? C45 C46 C48 111.3(7) . . ? C45 C46 C47 110.8(7) . . ? C48 C46 C47 109.7(7) . . ? C41 C49 C51 112.3(7) . . ? C41 C49 C50 110.4(7) . . ? C51 C49 C50 109.9(7) . . ? O8 C53 C54 122.9(7) . . ? O8 C53 C52 116.7(7) . . ? C54 C53 C52 120.3(7) . . ? C53 C54 C55 125.0(7) . . ? N3 C55 C54 124.9(8) . . ? N3 C55 C56 120.3(8) . . ? C54 C55 C56 114.8(7) . . ? C62 C57 C58 122.9(7) . . ? C62 C57 N3 118.8(7) . . ? C58 C57 N3 118.2(8) . . ? C59 C58 C57 116.3(8) . . ? C59 C58 C66 120.4(8) . . ? C57 C58 C66 123.3(7) . . ? C60 C59 C58 122.6(8) . . ? C59 C60 C61 119.6(8) . . ? C60 C61 C62 121.8(8) . . ? C57 C62 C61 116.7(8) . . ? C57 C62 C63 124.2(7) . . ? C61 C62 C63 119.1(8) . . ? C62 C63 C64 112.1(7) . . ? C62 C63 C65 112.4(7) . . ? C64 C63 C65 108.5(7) . . ? C58 C66 C68 111.7(7) . . ? C58 C66 C67 111.3(7) . . ? C68 C66 C67 110.7(8) . . ? 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 O2 Mo1 N1 C21 -100.0(9) . . . . ? O1 Mo1 N1 C21 156.1(9) . . . . ? O4 Mo1 N1 C21 -10.4(8) . . . . ? O3 Mo1 N1 C21 67.1(9) . . . . ? N2 Mo1 N1 C21 50.8(18) . . . . ? O2 Mo1 N1 C23 79.5(7) . . . . ? O1 Mo1 N1 C23 -24.3(7) . . . . ? O4 Mo1 N1 C23 169.1(7) . . . . ? O3 Mo1 N1 C23 -113.3(7) . . . . ? N2 Mo1 N1 C23 -129.7(15) . . . . ? O2 Mo1 N2 C4 -163.5(8) . . . . ? O1 Mo1 N2 C4 -59.5(8) . . . . ? O4 Mo1 N2 C4 105.3(8) . . . . ? O3 Mo1 N2 C4 28.6(8) . . . . ? N1 Mo1 N2 C4 45.1(19) . . . . ? O2 Mo1 N2 C6 8.8(7) . . . . ? O1 Mo1 N2 C6 112.8(7) . . . . ? O4 Mo1 N2 C6 -82.4(7) . . . . ? O3 Mo1 N2 C6 -159.1(7) . . . . ? N1 Mo1 N2 C6 -142.6(13) . . . . ? O5 Mo2 N3 C55 -98.9(9) . . . . ? O6 Mo2 N3 C55 157.8(9) . . . . ? O8 Mo2 N3 C55 -8.6(8) . . . . ? O7 Mo2 N3 C55 68.2(8) . . . . ? N4 Mo2 N3 C55 52.5(16) . . . . ? O5 Mo2 N3 C57 79.0(7) . . . . ? O6 Mo2 N3 C57 -24.4(6) . . . . ? O8 Mo2 N3 C57 169.3(7) . . . . ? O7 Mo2 N3 C57 -113.9(6) . . . . ? N4 Mo2 N3 C57 -129.7(13) . . . . ? O5 Mo2 N4 C38 -161.4(9) . . . . ? O6 Mo2 N4 C38 -57.8(8) . . . . ? O8 Mo2 N4 C38 106.5(8) . . . . ? O7 Mo2 N4 C38 30.7(8) . . . . ? N3 Mo2 N4 C38 46.7(17) . . . . ? O5 Mo2 N4 C40 9.1(7) . . . . ? O6 Mo2 N4 C40 112.6(7) . . . . ? O8 Mo2 N4 C40 -83.0(7) . . . . ? O7 Mo2 N4 C40 -158.8(7) . . . . ? N3 Mo2 N4 C40 -142.9(11) . . . . ? O2 Mo1 O3 C2 -84.1(12) . . . . ? O1 Mo1 O3 C2 59.6(7) . . . . ? O4 Mo1 O3 C2 -132.8(7) . . . . ? N2 Mo1 O3 C2 -36.0(7) . . . . ? N1 Mo1 O3 C2 146.7(7) . . . . ? O2 Mo1 O4 C19 118.0(8) . . . . ? O1 Mo1 O4 C19 -30.9(14) . . . . ? O3 Mo1 O4 C19 -74.3(8) . . . . ? N2 Mo1 O4 C19 -154.4(8) . . . . ? N1 Mo1 O4 C19 17.2(8) . . . . ? O5 Mo2 O7 C36 -87.6(12) . . . . ? O6 Mo2 O7 C36 58.4(6) . . . . ? O8 Mo2 O7 C36 -133.1(6) . . . . ? N4 Mo2 O7 C36 -37.3(6) . . . . ? N3 Mo2 O7 C36 145.9(6) . . . . ? O5 Mo2 O8 C53 117.2(8) . . . . ? O6 Mo2 O8 C53 -33.7(14) . . . . ? O7 Mo2 O8 C53 -74.0(8) . . . . ? N4 Mo2 O8 C53 -153.8(8) . . . . ? N3 Mo2 O8 C53 16.0(8) . . . . ? Mo1 O3 C2 C3 25.1(11) . . . . ? Mo1 O3 C2 C1 -157.6(5) . . . . ? O3 C2 C3 C4 7.9(12) . . . . ? C1 C2 C3 C4 -169.3(7) . . . . ? C6 N2 C4 C3 174.1(7) . . . . ? Mo1 N2 C4 C3 -13.5(12) . . . . ? C6 N2 C4 C5 -6.9(12) . . . . ? Mo1 N2 C4 C5 165.5(6) . . . . ? C2 C3 C4 N2 -13.0(12) . . . . ? C2 C3 C4 C5 167.9(7) . . . . ? C4 N2 C6 C7 -94.6(9) . . . . ? Mo1 N2 C6 C7 92.4(8) . . . . ? C4 N2 C6 C11 88.1(10) . . . . ? Mo1 N2 C6 C11 -84.9(8) . . . . ? C11 C6 C7 C8 0.5(11) . . . . ? N2 C6 C7 C8 -176.6(8) . . . . ? C11 C6 C7 C15 -178.9(7) . . . . ? N2 C6 C7 C15 4.0(12) . . . . ? C6 C7 C8 C9 1.2(11) . . . . ? C15 C7 C8 C9 -179.3(7) . . . . ? C7 C8 C9 C10 -2.5(12) . . . . ? C8 C9 C10 C11 2.2(13) . . . . ? C7 C6 C11 C10 -0.9(12) . . . . ? N2 C6 C11 C10 176.2(8) . . . . ? C7 C6 C11 C12 178.3(7) . . . . ? N2 C6 C11 C12 -4.6(13) . . . . ? C9 C10 C11 C6 -0.5(12) . . . . ? C9 C10 C11 C12 -179.7(8) . . . . ? C6 C11 C12 C13 -122.9(9) . . . . ? C10 C11 C12 C13 56.2(10) . . . . ? C6 C11 C12 C14 113.3(9) . . . . ? C10 C11 C12 C14 -67.6(10) . . . . ? C6 C7 C15 C16 -130.9(8) . . . . ? C8 C7 C15 C16 49.6(10) . . . . ? C6 C7 C15 C17 105.8(9) . . . . ? C8 C7 C15 C17 -73.7(9) . . . . ? Mo1 O4 C19 C20 -15.1(13) . . . . ? Mo1 O4 C19 C18 167.4(6) . . . . ? O4 C19 C20 C21 -0.6(13) . . . . ? C18 C19 C20 C21 176.8(8) . . . . ? C23 N1 C21 C20 -176.1(7) . . . . ? Mo1 N1 C21 C20 3.4(13) . . . . ? C23 N1 C21 C22 5.6(13) . . . . ? Mo1 N1 C21 C22 -174.9(6) . . . . ? C19 C20 C21 N1 5.5(13) . . . . ? C19 C20 C21 C22 -176.1(8) . . . . ? C21 N1 C23 C24 -88.3(10) . . . . ? Mo1 N1 C23 C24 92.1(8) . . . . ? C21 N1 C23 C28 92.0(10) . . . . ? Mo1 N1 C23 C28 -87.6(8) . . . . ? C28 C23 C24 C25 0.3(11) . . . . ? N1 C23 C24 C25 -179.5(8) . . . . ? C28 C23 C24 C32 179.0(7) . . . . ? N1 C23 C24 C32 -0.7(12) . . . . ? C23 C24 C25 C26 0.1(12) . . . . ? C32 C24 C25 C26 -178.8(7) . . . . ? C24 C25 C26 C27 0.7(13) . . . . ? C25 C26 C27 C28 -1.8(13) . . . . ? C26 C27 C28 C23 2.1(11) . . . . ? C26 C27 C28 C29 -175.7(8) . . . . ? C24 C23 C28 C27 -1.3(11) . . . . ? N1 C23 C28 C27 178.5(7) . . . . ? C24 C23 C28 C29 176.4(7) . . . . ? N1 C23 C28 C29 -3.8(11) . . . . ? C27 C28 C29 C30 -54.8(10) . . . . ? C23 C28 C29 C30 127.6(8) . . . . ? C27 C28 C29 C31 67.2(10) . . . . ? C23 C28 C29 C31 -110.4(8) . . . . ? C23 C24 C32 C33 118.1(8) . . . . ? C25 C24 C32 C33 -63.1(9) . . . . ? C23 C24 C32 C34 -119.4(8) . . . . ? C25 C24 C32 C34 59.4(10) . . . . ? Mo2 O7 C36 C37 26.4(10) . . . . ? Mo2 O7 C36 C35 -157.0(5) . . . . ? O7 C36 C37 C38 6.7(12) . . . . ? C35 C36 C37 C38 -169.8(7) . . . . ? C40 N4 C38 C37 173.5(8) . . . . ? Mo2 N4 C38 C37 -16.1(13) . . . . ? C40 N4 C38 C39 -6.6(13) . . . . ? Mo2 N4 C38 C39 163.8(6) . . . . ? C36 C37 C38 N4 -11.4(13) . . . . ? C36 C37 C38 C39 168.6(7) . . . . ? C38 N4 C40 C41 -93.1(10) . . . . ? Mo2 N4 C40 C41 95.8(8) . . . . ? C38 N4 C40 C45 89.6(11) . . . . ? Mo2 N4 C40 C45 -81.5(9) . . . . ? C45 C40 C41 C42 1.8(12) . . . . ? N4 C40 C41 C42 -175.4(8) . . . . ? C45 C40 C41 C49 -177.7(7) . . . . ? N4 C40 C41 C49 5.1(12) . . . . ? C40 C41 C42 C43 -1.0(12) . . . . ? C49 C41 C42 C43 178.6(7) . . . . ? C41 C42 C43 C44 -0.2(12) . . . . ? C42 C43 C44 C45 0.6(13) . . . . ? C43 C44 C45 C40 0.2(12) . . . . ? C43 C44 C45 C46 -176.8(8) . . . . ? C41 C40 C45 C44 -1.4(12) . . . . ? N4 C40 C45 C44 175.8(8) . . . . ? C41 C40 C45 C46 175.4(8) . . . . ? N4 C40 C45 C46 -7.4(13) . . . . ? C44 C45 C46 C48 56.1(10) . . . . ? C40 C45 C46 C48 -120.7(9) . . . . ? C44 C45 C46 C47 -66.3(10) . . . . ? C40 C45 C46 C47 117.0(9) . . . . ? C42 C41 C49 C51 52.0(10) . . . . ? C40 C41 C49 C51 -128.5(8) . . . . ? C42 C41 C49 C50 -71.1(10) . . . . ? C40 C41 C49 C50 108.4(9) . . . . ? Mo2 O8 C53 C54 -14.5(12) . . . . ? Mo2 O8 C53 C52 167.7(6) . . . . ? O8 C53 C54 C55 -0.6(13) . . . . ? C52 C53 C54 C55 177.1(8) . . . . ? C57 N3 C55 C54 -176.7(8) . . . . ? Mo2 N3 C55 C54 1.1(13) . . . . ? C57 N3 C55 C56 4.4(12) . . . . ? Mo2 N3 C55 C56 -177.8(7) . . . . ? C53 C54 C55 N3 6.6(13) . . . . ? C53 C54 C55 C56 -174.4(8) . . . . ? C55 N3 C57 C62 -90.4(10) . . . . ? Mo2 N3 C57 C62 91.5(8) . . . . ? C55 N3 C57 C58 88.9(10) . . . . ? Mo2 N3 C57 C58 -89.2(8) . . . . ? C62 C57 C58 C59 -0.5(11) . . . . ? N3 C57 C58 C59 -179.8(7) . . . . ? C62 C57 C58 C66 178.2(7) . . . . ? N3 C57 C58 C66 -1.1(12) . . . . ? C57 C58 C59 C60 0.5(12) . . . . ? C66 C58 C59 C60 -178.2(8) . . . . ? C58 C59 C60 C61 0.4(12) . . . . ? C59 C60 C61 C62 -1.5(12) . . . . ? C58 C57 C62 C61 -0.5(11) . . . . ? N3 C57 C62 C61 178.8(8) . . . . ? C58 C57 C62 C63 -179.7(7) . . . . ? N3 C57 C62 C63 -0.4(12) . . . . ? C60 C61 C62 C57 1.5(12) . . . . ? C60 C61 C62 C63 -179.2(7) . . . . ? C57 C62 C63 C64 115.6(9) . . . . ? C61 C62 C63 C64 -63.6(10) . . . . ? C57 C62 C63 C65 -121.9(8) . . . . ? C61 C62 C63 C65 58.9(9) . . . . ? C59 C58 C66 C68 -57.8(10) . . . . ? C57 C58 C66 C68 123.5(9) . . . . ? C59 C58 C66 C67 66.5(10) . . . . ? C57 C58 C66 C67 -112.2(9) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.36 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.928 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.162 # Attachment 'complex_4.cif' data_gru _database_code_depnum_ccdc_archive 'CCDC 695782' _chemical_compound_source 'synthetical product' _chemical_name_systematic ; di[4-(phenylimino)-2-pentanonato-N,O]dioxo molybdenum ; _chemical_name_common 'di(4-(phenylimino)-2-pentanonato-N,O)dioxo molybdenum' _chemical_melting_point ? _chemical_formula_moiety 'C22 H24 Mo N2 O4' _chemical_formula_sum 'C22 H24 Mo N2 O4' _chemical_formula_weight 476.37 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' 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 monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _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 11.249(2) _cell_length_b 9.8926(18) _cell_length_c 19.152(4) _cell_angle_alpha 90.00 _cell_angle_beta 92.651(17) _cell_angle_gamma 90.00 _cell_volume 2129.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 95(2) _cell_measurement_reflns_used 73 _cell_measurement_theta_min 19.14 _cell_measurement_theta_max 19.85 _exptl_crystal_description cube _exptl_crystal_colour 'dark yellow' _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.486 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 976 _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8232 _exptl_absorpt_correction_T_max 0.9233 _exptl_absorpt_process_details 'Parkin, S., Moezzi, B. and Hope H. (1995) J. Appl. Cryst. 28, 53-56' _exptl_special_details ; ? ; _diffrn_ambient_temperature 95(2) _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type Stoe _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method '\w-\q scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 7341 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0660 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 30.00 _reflns_number_total 6199 _reflns_number_gt 5006 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'local software' _computing_cell_refinement 'local software' _computing_data_reduction 'local software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1965)' _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. The non-hydrogen atoms were refined with anisotropic displacement parameters without any constraints. The H atoms H13 and H33 were put at the external bisector of the C-C-C angle at a C-H distance of 0.95 \%A but the individual isotropic displacement parameters are free to refine (AFIX 43 of SHELXL-97). The C atoms of the phenyl rings were refined without any constraints. The H atoms were put at the external bisector of the C-C-C angle at a C-H distance of 0.95 \%A and common isotropic displacement parameters were refined for the H atoms of the same phenyl group (AFIX 43 of SHELXL-97). The H atoms of the methyl groups were refined with common isotropic displacement parameters for the H atoms of the same group and idealized geometry with tetrahedral angles, enabling rotation around the X-C bond, and C-H distances of 0.98 \%A (AFIX 137 of SHELXL-97). ; _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^)+(0.0561P)^2^+1.0100P] 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 refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6199 _refine_ls_number_parameters 274 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1268 _refine_ls_wR_factor_gt 0.1161 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _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 0.74914(2) 0.74069(2) 0.506987(12) 0.01518(8) Uani 1 1 d . . . O1 O 0.59795(18) 0.7304(2) 0.51077(11) 0.0187(4) Uani 1 1 d . . . O3 O 0.80340(18) 0.6214(2) 0.56486(10) 0.0198(4) Uani 1 1 d . . . C11 C 1.1237(3) 0.7072(3) 0.47190(18) 0.0254(6) Uani 1 1 d . . . H111 H 1.1486 0.7884 0.4471 0.061(8) Uiso 1 1 calc R . . H112 H 1.1694 0.6293 0.4565 0.061(8) Uiso 1 1 calc R . . H113 H 1.1379 0.7201 0.5223 0.061(8) Uiso 1 1 calc R . . C12 C 0.9941(3) 0.6828(3) 0.45618(15) 0.0194(6) Uani 1 1 d . . . O12 O 0.92331(19) 0.7776(2) 0.47505(11) 0.0200(4) Uani 1 1 d . . . C13 C 0.9554(3) 0.5675(3) 0.42108(14) 0.0193(6) Uani 1 1 d . . . H13 H 1.0121 0.4982 0.4142 0.030(10) Uiso 1 1 calc R . . C14 C 0.8384(3) 0.5456(3) 0.39488(14) 0.0178(5) Uani 1 1 d . . . C15 C 0.8206(3) 0.4385(3) 0.33968(16) 0.0240(6) Uani 1 1 d . . . H151 H 0.7486 0.3865 0.3484 0.041(7) Uiso 1 1 calc R . . H152 H 0.8895 0.3778 0.3411 0.041(7) Uiso 1 1 calc R . . H153 H 0.8120 0.4813 0.2936 0.041(7) Uiso 1 1 calc R . . N14 N 0.7454(2) 0.6168(2) 0.41570(12) 0.0170(5) Uani 1 1 d . . . C21 C 0.6336(2) 0.6036(3) 0.37614(15) 0.0180(5) Uani 1 1 d . . . C22 C 0.6121(3) 0.6844(3) 0.31754(15) 0.0209(6) Uani 1 1 d . . . H22 H 0.6697 0.7487 0.3044 0.036(5) Uiso 1 1 calc R . . C23 C 0.5059(3) 0.6706(3) 0.27824(16) 0.0246(6) Uani 1 1 d . . . H23 H 0.4915 0.7247 0.2377 0.036(5) Uiso 1 1 calc R . . C24 C 0.4208(3) 0.5783(4) 0.29780(17) 0.0277(7) Uani 1 1 d . . . H24 H 0.3488 0.5683 0.2704 0.036(5) Uiso 1 1 calc R . . C25 C 0.4413(3) 0.5006(4) 0.35757(17) 0.0280(7) Uani 1 1 d . . . H25 H 0.3824 0.4388 0.3717 0.036(5) Uiso 1 1 calc R . . C26 C 0.5481(3) 0.5132(3) 0.39685(16) 0.0237(6) Uani 1 1 d . . . H26 H 0.5622 0.4600 0.4377 0.036(5) Uiso 1 1 calc R . . C31 C 0.6065(3) 1.0964(3) 0.39685(15) 0.0231(6) Uani 1 1 d . . . H311 H 0.6710 1.1418 0.3733 0.037(6) Uiso 1 1 calc R . . H312 H 0.5521 1.1643 0.4146 0.037(6) Uiso 1 1 calc R . . H313 H 0.5630 1.0371 0.3636 0.037(6) Uiso 1 1 calc R . . C32 C 0.6580(2) 1.0138(3) 0.45665(14) 0.0171(5) Uani 1 1 d . . . O32 O 0.72325(19) 0.9136(2) 0.44041(10) 0.0201(4) Uani 1 1 d . . . C33 C 0.6389(2) 1.0535(3) 0.52528(14) 0.0179(5) Uani 1 1 d . . . H33 H 0.5758 1.1147 0.5331 0.036(11) Uiso 1 1 calc R . . C34 C 0.7082(3) 1.0073(3) 0.58298(14) 0.0175(5) Uani 1 1 d . . . C35 C 0.7050(3) 1.0875(3) 0.65007(15) 0.0234(6) Uani 1 1 d . . . H351 H 0.6766 1.0295 0.6873 0.043(7) Uiso 1 1 calc R . . H352 H 0.6511 1.1647 0.6432 0.043(7) Uiso 1 1 calc R . . H353 H 0.7851 1.1202 0.6632 0.043(7) Uiso 1 1 calc R . . N34 N 0.7771(2) 0.8968(3) 0.58158(12) 0.0170(5) Uani 1 1 d . . . C41 C 0.8718(3) 0.8820(3) 0.63415(14) 0.0170(5) Uani 1 1 d . . . C42 C 0.8581(3) 0.7988(3) 0.69214(15) 0.0215(6) Uani 1 1 d . . . H42 H 0.7871 0.7479 0.6963 0.030(5) Uiso 1 1 calc R . . C43 C 0.9489(3) 0.7909(3) 0.74366(15) 0.0246(6) Uani 1 1 d . . . H43 H 0.9392 0.7355 0.7835 0.030(5) Uiso 1 1 calc R . . C44 C 1.0536(3) 0.8633(3) 0.73743(16) 0.0252(7) Uani 1 1 d . . . H44 H 1.1144 0.8594 0.7735 0.030(5) Uiso 1 1 calc R . . C45 C 1.0693(3) 0.9414(3) 0.67836(17) 0.0246(6) Uani 1 1 d . . . H45 H 1.1420 0.9886 0.6732 0.030(5) Uiso 1 1 calc R . . C46 C 0.9785(3) 0.9505(3) 0.62656(15) 0.0208(6) Uani 1 1 d . . . H46 H 0.9894 1.0035 0.5860 0.030(5) 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 0.01586(13) 0.01531(13) 0.01425(12) -0.00109(9) -0.00061(8) 0.00126(9) O1 0.0176(10) 0.0192(10) 0.0193(10) -0.0023(8) 0.0002(7) 0.0009(8) O3 0.0223(10) 0.0209(10) 0.0160(9) -0.0018(8) -0.0011(8) 0.0032(8) C11 0.0174(14) 0.0259(15) 0.0325(17) 0.0045(13) -0.0021(12) -0.0012(12) C12 0.0235(14) 0.0197(13) 0.0153(12) 0.0043(10) 0.0035(10) 0.0017(11) O12 0.0191(10) 0.0180(10) 0.0227(10) -0.0014(8) 0.0009(8) 0.0001(8) C13 0.0199(13) 0.0213(14) 0.0168(12) 0.0020(11) 0.0003(10) 0.0025(11) C14 0.0211(13) 0.0176(13) 0.0146(12) 0.0024(10) 0.0006(10) 0.0034(11) C15 0.0268(15) 0.0217(15) 0.0232(14) -0.0046(12) -0.0010(12) 0.0042(12) N14 0.0188(11) 0.0168(11) 0.0152(11) -0.0003(9) -0.0014(9) -0.0005(9) C21 0.0161(13) 0.0210(14) 0.0168(12) -0.0035(10) 0.0002(10) 0.0008(11) C22 0.0228(14) 0.0224(14) 0.0175(13) -0.0015(11) 0.0021(11) 0.0001(12) C23 0.0263(15) 0.0304(17) 0.0168(13) -0.0040(12) -0.0034(11) 0.0050(13) C24 0.0198(14) 0.0405(19) 0.0226(15) -0.0085(14) -0.0026(11) 0.0000(14) C25 0.0248(16) 0.0317(17) 0.0276(16) -0.0042(13) 0.0033(13) -0.0112(13) C26 0.0254(15) 0.0245(15) 0.0209(14) 0.0002(12) -0.0010(12) -0.0026(12) C31 0.0257(15) 0.0241(15) 0.0196(13) 0.0050(11) 0.0011(11) 0.0047(12) C32 0.0164(12) 0.0177(13) 0.0168(12) 0.0013(10) -0.0024(10) -0.0038(10) O32 0.0233(10) 0.0214(10) 0.0157(9) 0.0007(8) -0.0003(8) 0.0030(8) C33 0.0165(12) 0.0186(13) 0.0184(13) 0.0005(10) 0.0009(10) 0.0006(11) C34 0.0178(13) 0.0191(13) 0.0157(12) -0.0014(10) 0.0012(10) -0.0015(11) C35 0.0279(15) 0.0245(15) 0.0178(13) -0.0045(11) -0.0004(11) 0.0066(12) N34 0.0172(11) 0.0187(11) 0.0150(10) -0.0007(9) -0.0016(9) -0.0002(9) C41 0.0194(13) 0.0183(13) 0.0130(12) -0.0027(10) -0.0023(10) 0.0019(11) C42 0.0263(15) 0.0222(14) 0.0158(13) -0.0007(11) -0.0004(11) -0.0007(12) C43 0.0334(17) 0.0253(15) 0.0145(13) 0.0001(11) -0.0046(12) 0.0058(13) C44 0.0264(16) 0.0278(16) 0.0206(14) -0.0057(12) -0.0075(12) 0.0086(13) C45 0.0207(14) 0.0253(15) 0.0274(15) -0.0052(12) -0.0039(12) 0.0015(12) C46 0.0245(14) 0.0180(13) 0.0198(13) -0.0005(11) -0.0009(11) -0.0006(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.709(2) . yes Mo1 O3 1.712(2) . yes Mo1 O12 2.111(2) . yes Mo1 N34 2.117(2) . yes Mo1 N14 2.134(2) . yes Mo1 O32 2.145(2) . yes C11 C12 1.494(4) . ? C11 H111 0.98 . ? C11 H112 0.98 . ? C11 H113 0.98 . ? C12 O12 1.293(4) . yes C12 C13 1.384(4) . ? C13 C14 1.404(4) . ? C13 H13 0.95 . ? C14 N14 1.337(4) . yes C14 C15 1.504(4) . ? C15 H151 0.98 . ? C15 H152 0.98 . ? C15 H153 0.98 . ? N14 C21 1.444(4) . yes C21 C26 1.385(4) . ? C21 C22 1.390(4) . ? C22 C23 1.389(4) . ? C22 H22 0.95 . ? C23 C24 1.387(5) . ? C23 H23 0.95 . ? C24 C25 1.389(5) . ? C24 H24 0.95 . ? C25 C26 1.394(4) . ? C25 H25 0.95 . ? C26 H26 0.95 . ? C31 C32 1.501(4) . ? C31 H311 0.98 . ? C31 H312 0.98 . ? C31 H313 0.98 . ? C32 O32 1.280(3) . yes C32 C33 1.398(4) . ? C33 C34 1.399(4) . ? C33 H33 0.95 . ? C34 N34 1.341(4) . yes C34 C35 1.512(4) . ? C35 H351 0.98 . ? C35 H352 0.98 . ? C35 H353 0.98 . ? N34 C41 1.439(3) . yes C41 C46 1.391(4) . ? C41 C42 1.397(4) . ? C42 C43 1.389(4) . ? C42 H42 0.95 . ? C43 C44 1.389(5) . ? C43 H43 0.95 . ? C44 C45 1.388(5) . ? C44 H44 0.95 . ? C45 C46 1.394(4) . ? C45 H45 0.95 . ? C46 H46 0.95 . ? 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 Mo1 O3 104.91(10) . . yes O1 Mo1 O12 164.05(9) . . yes O3 Mo1 O12 89.94(9) . . ? O1 Mo1 N34 97.57(9) . . yes O3 Mo1 N34 91.64(10) . . ? O12 Mo1 N34 87.63(9) . . ? O1 Mo1 N14 91.08(10) . . ? O3 Mo1 N14 97.31(10) . . yes O12 Mo1 N14 81.09(9) . . yes N34 Mo1 N14 165.56(9) . . yes O1 Mo1 O32 87.97(9) . . ? O3 Mo1 O32 165.68(9) . . yes O12 Mo1 O32 78.00(8) . . yes N34 Mo1 O32 80.29(9) . . yes N14 Mo1 O32 88.52(9) . . ? C12 C11 H111 109.5 . . ? C12 C11 H112 109.5 . . ? H111 C11 H112 109.5 . . ? C12 C11 H113 109.5 . . ? H111 C11 H113 109.5 . . ? H112 C11 H113 109.5 . . ? O12 C12 C13 123.3(3) . . ? O12 C12 C11 115.7(3) . . ? C13 C12 C11 120.9(3) . . ? C12 O12 Mo1 123.21(19) . . ? C12 C13 C14 124.7(3) . . ? C12 C13 H13 117.6 . . ? C14 C13 H13 117.6 . . ? N14 C14 C13 123.1(3) . . ? N14 C14 C15 120.0(3) . . ? C13 C14 C15 116.9(3) . . ? C14 C15 H151 109.5 . . ? C14 C15 H152 109.5 . . ? H151 C15 H152 109.5 . . ? C14 C15 H153 109.5 . . ? H151 C15 H153 109.5 . . ? H152 C15 H153 109.5 . . ? C14 N14 C21 118.1(2) . . yes C14 N14 Mo1 124.13(19) . . yes C21 N14 Mo1 117.71(18) . . yes C26 C21 C22 120.3(3) . . ? C26 C21 N14 120.5(3) . . ? C22 C21 N14 119.2(3) . . ? C23 C22 C21 119.7(3) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 C22 120.4(3) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C23 C24 C25 119.8(3) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 120.1(3) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 119.8(3) . . ? C21 C26 H26 120.1 . . ? C25 C26 H26 120.1 . . ? C32 C31 H311 109.5 . . ? C32 C31 H312 109.5 . . ? H311 C31 H312 109.5 . . ? C32 C31 H313 109.5 . . ? H311 C31 H313 109.5 . . ? H312 C31 H313 109.5 . . ? O32 C32 C33 124.1(3) . . ? O32 C32 C31 116.2(2) . . ? C33 C32 C31 119.6(3) . . ? C32 O32 Mo1 122.44(18) . . ? C32 C33 C34 123.2(3) . . ? C32 C33 H33 118.4 . . ? C34 C33 H33 118.4 . . ? N34 C34 C33 123.5(3) . . ? N34 C34 C35 118.8(3) . . ? C33 C34 C35 117.8(3) . . ? C34 C35 H351 109.5 . . ? C34 C35 H352 109.5 . . ? H351 C35 H352 109.5 . . ? C34 C35 H353 109.5 . . ? H351 C35 H353 109.5 . . ? H352 C35 H353 109.5 . . ? C34 N34 C41 118.6(2) . . yes C34 N34 Mo1 122.71(19) . . yes C41 N34 Mo1 118.69(18) . . yes C46 C41 C42 119.9(3) . . ? C46 C41 N34 119.5(3) . . ? C42 C41 N34 120.7(3) . . ? C43 C42 C41 119.5(3) . . ? C43 C42 H42 120.2 . . ? C41 C42 H42 120.2 . . ? C44 C43 C42 120.6(3) . . ? C44 C43 H43 119.7 . . ? C42 C43 H43 119.7 . . ? C45 C44 C43 119.8(3) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C45 C46 119.9(3) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C41 C46 C45 120.1(3) . . ? C41 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? 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 C13 C12 O12 Mo1 34.2(4) . . . . ? C11 C12 O12 Mo1 -148.3(2) . . . . ? O1 Mo1 O12 C12 -107.6(4) . . . . ? O3 Mo1 O12 C12 51.2(2) . . . . ? N34 Mo1 O12 C12 142.8(2) . . . . ? N14 Mo1 O12 C12 -46.2(2) . . . . ? O32 Mo1 O12 C12 -136.6(2) . . . . ? O12 C12 C13 C14 7.4(5) . . . . ? C11 C12 C13 C14 -169.9(3) . . . . ? C12 C13 C14 N14 -17.5(4) . . . . ? C12 C13 C14 C15 161.1(3) . . . . ? C13 C14 N14 C21 168.4(3) . . . . ? C15 C14 N14 C21 -10.0(4) . . . . ? C13 C14 N14 Mo1 -15.0(4) . . . . ? C15 C14 N14 Mo1 166.5(2) . . . . ? O1 Mo1 N14 C14 -157.5(2) . . . . ? O3 Mo1 N14 C14 -52.3(2) . . . . ? O12 Mo1 N14 C14 36.5(2) . . . . ? N34 Mo1 N14 C14 75.5(4) . . . . ? O32 Mo1 N14 C14 114.6(2) . . . . ? O1 Mo1 N14 C21 19.1(2) . . . . ? O3 Mo1 N14 C21 124.3(2) . . . . ? O12 Mo1 N14 C21 -147.0(2) . . . . ? N34 Mo1 N14 C21 -107.9(4) . . . . ? O32 Mo1 N14 C21 -68.9(2) . . . . ? C14 N14 C21 C26 95.3(3) . . . . ? Mo1 N14 C21 C26 -81.5(3) . . . . ? C14 N14 C21 C22 -85.7(3) . . . . ? Mo1 N14 C21 C22 97.5(3) . . . . ? C26 C21 C22 C23 -2.3(4) . . . . ? N14 C21 C22 C23 178.6(3) . . . . ? C21 C22 C23 C24 1.0(5) . . . . ? C22 C23 C24 C25 0.9(5) . . . . ? C23 C24 C25 C26 -1.4(5) . . . . ? C22 C21 C26 C25 1.8(5) . . . . ? N14 C21 C26 C25 -179.2(3) . . . . ? C24 C25 C26 C21 0.1(5) . . . . ? C33 C32 O32 Mo1 28.7(4) . . . . ? C31 C32 O32 Mo1 -155.3(2) . . . . ? O1 Mo1 O32 C32 51.2(2) . . . . ? O3 Mo1 O32 C32 -103.3(4) . . . . ? O12 Mo1 O32 C32 -136.5(2) . . . . ? N34 Mo1 O32 C32 -46.8(2) . . . . ? N14 Mo1 O32 C32 142.3(2) . . . . ? O32 C32 C33 C34 14.2(5) . . . . ? C31 C32 C33 C34 -161.7(3) . . . . ? C32 C33 C34 N34 -18.2(5) . . . . ? C32 C33 C34 C35 161.5(3) . . . . ? C33 C34 N34 C41 160.2(3) . . . . ? C35 C34 N34 C41 -19.5(4) . . . . ? C33 C34 N34 Mo1 -21.5(4) . . . . ? C35 C34 N34 Mo1 158.7(2) . . . . ? O1 Mo1 N34 C34 -43.9(2) . . . . ? O3 Mo1 N34 C34 -149.2(2) . . . . ? O12 Mo1 N34 C34 120.9(2) . . . . ? N14 Mo1 N34 C34 82.4(4) . . . . ? O32 Mo1 N34 C34 42.7(2) . . . . ? O1 Mo1 N34 C41 134.3(2) . . . . ? O3 Mo1 N34 C41 29.0(2) . . . . ? O12 Mo1 N34 C41 -60.8(2) . . . . ? N14 Mo1 N34 C41 -99.4(4) . . . . ? O32 Mo1 N34 C41 -139.1(2) . . . . ? C34 N34 C41 C46 -80.3(3) . . . . ? Mo1 N34 C41 C46 101.3(3) . . . . ? C34 N34 C41 C42 100.3(3) . . . . ? Mo1 N34 C41 C42 -78.0(3) . . . . ? C46 C41 C42 C43 3.5(4) . . . . ? N34 C41 C42 C43 -177.2(3) . . . . ? C41 C42 C43 C44 -1.0(5) . . . . ? C42 C43 C44 C45 -1.8(5) . . . . ? C43 C44 C45 C46 2.1(5) . . . . ? C42 C41 C46 C45 -3.1(4) . . . . ? N34 C41 C46 C45 177.5(3) . . . . ? C44 C45 C46 C41 0.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.671 _refine_diff_density_min -0.957 _refine_diff_density_rms 0.117 # Attachment '[{Li_LMe2Ph__LMe2PhH_}2].cif' data_[{Li(LMe2Ph)(LMe2PhH)}2] _database_code_depnum_ccdc_archive 'CCDC 708730' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H66 Li2 N4 O4' _chemical_formula_sum 'C52 H66 Li2 N4 O4' _chemical_formula_weight 824.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li 0.0008 0.0003 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.915(3) _cell_length_b 15.694(3) _cell_length_c 19.468(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.22(2) _cell_angle_gamma 90.00 _cell_volume 2411.7(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3446 _cell_measurement_theta_min 3.62 _cell_measurement_theta_max 59.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 0.550 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9074 _exptl_absorpt_correction_T_max 0.9701 _exptl_absorpt_process_details 'SADABS, Sheldrick 2007' _exptl_special_details ; The intensities were measured with Bruker Smart 6000 area CCD detector The geometry of the diffractometer allowed to collect data only to 0.9 \%A ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'mirror system' _diffrn_measurement_device_type 'Bruker three circle diffractometer' _diffrn_measurement_method 'phi and omega scan' _diffrn_detector_area_resol_mean 5.602 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10466 _diffrn_reflns_av_R_equivalents 0.0412 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 59.00 _reflns_number_total 3446 _reflns_number_gt 2710 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Proteum (v 1.40, Bruker 2002)' _computing_cell_refinement 'Bruker AXS SAINT (v 7.34A, Bruker 2003)' _computing_data_reduction 'Bruker AXS SAINT (v 7.34A, Bruker 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker AXS SHELXTL (v 6.12)' _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. One of the 2,6-dimethylphenyl rings is disordered with the ocupancy ratio of 64.9:35.1 %. The following restraints and constraints were used to treat the disorder: SIMU, DELU, SADI, SAME. Due to this large disorder (21% of the molecule) and the possibility to acheave only the resolution of 0.9 \%A, due to the geometry of the equippment, the data:parameter ratio (9.73) is slightly lower than the value of 10 requested by Acta Crystallographica. ; _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^)+(0.0618P)^2^+0.4136P] 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 3446 _refine_ls_number_parameters 354 _refine_ls_number_restraints 724 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1086 _refine_ls_wR_factor_gt 0.1011 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 0.953 _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 O1 O 0.09818(13) 0.06840(6) 0.98647(5) 0.0288(3) Uani 1 1 d . . . N1 N -0.11869(16) 0.14533(8) 1.08386(6) 0.0280(3) Uani 1 1 d D . . C1 C 0.2205(2) 0.16213(11) 0.90814(8) 0.0349(4) Uani 1 1 d . . . H1A H 0.3213 0.1257 0.9125 0.052 Uiso 1 1 calc R . . H1B H 0.2552 0.2221 0.9077 0.052 Uiso 1 1 calc R . . H1C H 0.1536 0.1487 0.8651 0.052 Uiso 1 1 calc R . . Li1 Li -0.0123(3) 0.03111(16) 1.06493(13) 0.0310(6) Uani 1 1 d . . . O2 O 0.08591(14) -0.00900(7) 1.15564(5) 0.0327(3) Uani 1 1 d . . . C2 C 0.1146(2) 0.14664(10) 0.96850(8) 0.0290(4) Uani 1 1 d . . . C3 C 0.0378(2) 0.21494(10) 0.99800(8) 0.0335(4) Uani 1 1 d . . . H3 H 0.0662 0.2695 0.9812 0.040 Uiso 1 1 calc R . . C4 C -0.0792(2) 0.21417(10) 1.05068(8) 0.0314(4) Uani 1 1 d D . . C5 C -0.1619(3) 0.29844(11) 1.06491(9) 0.0441(5) Uani 1 1 d . . . H5A H -0.2520 0.2895 1.0961 0.066 Uiso 0.50 1 calc PR . . H5B H -0.2104 0.3230 1.0215 0.066 Uiso 0.50 1 calc PR . . H5C H -0.0770 0.3375 1.0863 0.066 Uiso 0.50 1 calc PR . . H5D H -0.1076 0.3438 1.0399 0.066 Uiso 0.50 1 calc PR . . H5E H -0.1492 0.3104 1.1144 0.066 Uiso 0.50 1 calc PR . . H5F H -0.2826 0.2958 1.0497 0.066 Uiso 0.50 1 calc PR . . C6 C -0.2375(2) 0.15139(9) 1.13562(8) 0.0276(4) Uani 1 1 d D . . C7 C -0.1819(2) 0.17464(9) 1.20333(8) 0.0315(4) Uani 1 1 d D . . C8 C -0.3005(2) 0.17770(10) 1.25277(8) 0.0354(4) Uani 1 1 d D . . H8 H -0.2649 0.1942 1.2985 0.043 Uiso 1 1 calc R . . C9 C -0.4684(2) 0.15730(11) 1.23679(9) 0.0391(4) Uani 1 1 d D . . H9 H -0.5476 0.1600 1.2711 0.047 Uiso 1 1 calc R . . C10 C -0.5203(2) 0.13287(10) 1.17043(9) 0.0354(4) Uani 1 1 d D . . H10 H -0.6354 0.1179 1.1596 0.042 Uiso 1 1 calc R . . C11 C -0.4070(2) 0.12986(10) 1.11926(8) 0.0307(4) Uani 1 1 d D . . C12 C -0.4645(2) 0.10383(11) 1.04684(8) 0.0385(4) Uani 1 1 d D . . H12A H -0.4525 0.1521 1.0157 0.058 Uiso 1 1 calc R . . H12B H -0.5836 0.0862 1.0451 0.058 Uiso 1 1 calc R . . H12C H -0.3950 0.0562 1.0327 0.058 Uiso 1 1 calc R . . C13 C 0.0007(2) 0.19618(11) 1.22123(9) 0.0386(4) Uani 1 1 d D . . H13A H 0.0722 0.1487 1.2081 0.058 Uiso 1 1 calc R . . H13B H 0.0188 0.2062 1.2709 0.058 Uiso 1 1 calc R . . H13C H 0.0305 0.2477 1.1963 0.058 Uiso 1 1 calc R . . C14 C 0.2903(2) -0.10409(11) 1.11613(8) 0.0376(4) Uani 1 1 d . . . H14A H 0.2213 -0.1144 1.0730 0.056 Uiso 1 1 calc R . . H14B H 0.3451 -0.1573 1.1319 0.056 Uiso 1 1 calc R . . H14C H 0.3769 -0.0613 1.1084 0.056 Uiso 1 1 calc R . . C15 C 0.1796(2) -0.07252(10) 1.16964(8) 0.0299(4) Uani 1 1 d . . . C16 C 0.1842(2) -0.11416(10) 1.23429(8) 0.0313(4) Uani 1 1 d . . . H16 H 0.2539 -0.1633 1.2403 0.038 Uiso 1 1 calc R . . C18 C 0.1067(2) -0.13859(11) 1.35498(9) 0.0417(5) Uani 1 1 d . . . H18A H 0.1360 -0.1000 1.3936 0.062 Uiso 1 1 calc R . . H18B H 0.1941 -0.1826 1.3533 0.062 Uiso 1 1 calc R . . H18C H -0.0029 -0.1655 1.3612 0.062 Uiso 1 1 calc R . . C17 C 0.0958(2) -0.08906(10) 1.28892(8) 0.0299(4) Uani 1 1 d D A . N2 N -0.00368(17) -0.01974(8) 1.28481(7) 0.0316(3) Uani 1 1 d D . . H2 H -0.016(2) 0.0055(13) 1.2401(11) 0.057(6) Uiso 1 1 d . . . C19 C -0.1065(5) 0.0091(3) 1.3374(2) 0.0313(8) Uani 0.639(11) 1 d PDU A 1 C20 C -0.2771(5) -0.0127(3) 1.3339(2) 0.0343(8) Uani 0.639(11) 1 d PDU A 1 C21 C -0.3736(6) 0.0154(3) 1.3868(3) 0.0354(9) Uani 0.639(11) 1 d PDU A 1 H21A H -0.4906 0.0015 1.3857 0.043 Uiso 0.639(11) 1 calc PR A 1 C22 C -0.3004(8) 0.0634(3) 1.4407(3) 0.0365(10) Uani 0.639(11) 1 d PDU A 1 H22A H -0.3669 0.0817 1.4766 0.044 Uiso 0.639(11) 1 calc PR A 1 C23 C -0.1304(8) 0.0849(4) 1.4426(3) 0.0378(9) Uani 0.639(11) 1 d PDU A 1 H23A H -0.0822 0.1186 1.4795 0.045 Uiso 0.639(11) 1 calc PR A 1 C24 C -0.0288(7) 0.0580(6) 1.3914(4) 0.0345(9) Uani 0.639(11) 1 d PDU A 1 C25 C 0.1568(8) 0.0826(7) 1.3950(5) 0.0449(14) Uani 0.639(11) 1 d PDU A 1 H25A H 0.1969 0.0818 1.3485 0.067 Uiso 0.639(11) 1 calc PR A 1 H25B H 0.2226 0.0419 1.4242 0.067 Uiso 0.639(11) 1 calc PR A 1 H25C H 0.1708 0.1399 1.4145 0.067 Uiso 0.639(11) 1 calc PR A 1 C26 C -0.3535(7) -0.0619(5) 1.2733(3) 0.0386(13) Uani 0.639(11) 1 d PDU A 1 H26A H -0.4743 -0.0711 1.2786 0.058 Uiso 0.639(11) 1 calc PR A 1 H26B H -0.2963 -0.1171 1.2709 0.058 Uiso 0.639(11) 1 calc PR A 1 H26C H -0.3398 -0.0298 1.2309 0.058 Uiso 0.639(11) 1 calc PR A 1 C19A C -0.1153(7) 0.0052(5) 1.3378(3) 0.0331(13) Uani 0.361(11) 1 d PRDU A 2 C20A C -0.2868(7) -0.0180(5) 1.3231(3) 0.0326(13) Uani 0.361(11) 1 d PRDU A 2 C21A C -0.4038(7) 0.0051(5) 1.3694(3) 0.0343(13) Uani 0.361(11) 1 d PRDU A 2 H21B H -0.5190 -0.0115 1.3615 0.041 Uiso 0.361(11) 1 calc PR A 2 C22A C -0.3515(12) 0.0525(6) 1.4272(5) 0.0352(13) Uani 0.361(11) 1 d PDU A 2 H22B H -0.4321 0.0669 1.4591 0.042 Uiso 0.361(11) 1 calc PR A 2 C23A C -0.1866(13) 0.0794(7) 1.4397(5) 0.0353(13) Uani 0.361(11) 1 d PDU A 2 H23B H -0.1551 0.1127 1.4794 0.042 Uiso 0.361(11) 1 calc PR A 2 C24A C -0.0649(13) 0.0574(11) 1.3935(7) 0.0355(13) Uani 0.361(11) 1 d PDU A 2 C25A C 0.1155(14) 0.0874(10) 1.4030(7) 0.0361(19) Uani 0.361(11) 1 d PDU A 2 H25D H 0.1790 0.0654 1.3654 0.054 Uiso 0.361(11) 1 calc PR A 2 H25E H 0.1670 0.0665 1.4471 0.054 Uiso 0.361(11) 1 calc PR A 2 H25F H 0.1181 0.1498 1.4026 0.054 Uiso 0.361(11) 1 calc PR A 2 C26A C -0.3424(16) -0.0675(9) 1.2592(6) 0.040(2) Uani 0.361(11) 1 d PDU A 2 H26D H -0.2752 -0.1197 1.2575 0.060 Uiso 0.361(11) 1 calc PR A 2 H26E H -0.3258 -0.0327 1.2185 0.060 Uiso 0.361(11) 1 calc PR A 2 H26F H -0.4626 -0.0822 1.2601 0.060 Uiso 0.361(11) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0339(6) 0.0256(6) 0.0273(6) 0.0003(4) 0.0037(5) -0.0019(5) N1 0.0301(8) 0.0266(7) 0.0273(7) -0.0003(6) 0.0030(6) -0.0009(6) C1 0.0381(10) 0.0349(9) 0.0323(9) 0.0023(7) 0.0065(8) -0.0036(8) Li1 0.0346(15) 0.0302(14) 0.0285(13) -0.0007(11) 0.0044(12) 0.0005(11) O2 0.0372(7) 0.0315(6) 0.0293(6) 0.0013(5) 0.0010(5) 0.0027(5) C2 0.0308(9) 0.0291(9) 0.0267(8) 0.0024(7) -0.0013(7) -0.0037(7) C3 0.0429(10) 0.0230(8) 0.0351(9) 0.0047(7) 0.0068(8) -0.0045(7) C4 0.0378(10) 0.0257(8) 0.0304(8) 0.0004(7) 0.0017(8) -0.0018(7) C5 0.0627(13) 0.0287(9) 0.0427(10) 0.0044(8) 0.0161(9) 0.0050(8) C6 0.0351(10) 0.0196(7) 0.0284(8) -0.0001(6) 0.0052(7) 0.0020(7) C7 0.0411(10) 0.0219(8) 0.0313(9) -0.0015(7) 0.0011(8) 0.0022(7) C8 0.0527(12) 0.0272(9) 0.0265(8) -0.0020(7) 0.0038(8) 0.0033(8) C9 0.0485(12) 0.0338(9) 0.0368(10) 0.0025(8) 0.0154(9) 0.0081(8) C10 0.0344(10) 0.0331(9) 0.0393(10) 0.0014(8) 0.0069(8) 0.0026(7) C11 0.0338(10) 0.0271(8) 0.0314(9) 0.0002(7) 0.0035(7) 0.0017(7) C12 0.0352(10) 0.0452(10) 0.0347(9) -0.0011(8) 0.0007(8) -0.0037(8) C13 0.0466(11) 0.0339(9) 0.0344(9) -0.0046(7) -0.0029(8) -0.0054(8) C14 0.0391(10) 0.0428(10) 0.0311(9) -0.0001(8) 0.0042(8) 0.0036(8) C15 0.0285(9) 0.0291(9) 0.0317(9) -0.0019(7) -0.0013(7) -0.0020(7) C16 0.0323(9) 0.0297(8) 0.0317(9) 0.0014(7) 0.0019(7) 0.0034(7) C18 0.0525(12) 0.0374(10) 0.0355(9) 0.0074(8) 0.0061(9) 0.0088(8) C17 0.0305(9) 0.0302(9) 0.0286(8) 0.0010(7) -0.0003(7) -0.0022(7) N2 0.0365(8) 0.0316(7) 0.0269(7) 0.0021(6) 0.0045(6) 0.0036(6) C19 0.0414(15) 0.0248(15) 0.0283(15) 0.0049(13) 0.0071(14) 0.0052(14) C20 0.0420(16) 0.0271(15) 0.0343(15) 0.0044(13) 0.0065(14) 0.0063(14) C21 0.0401(17) 0.0315(16) 0.0354(18) 0.0035(14) 0.0065(15) 0.0030(14) C22 0.047(2) 0.0308(17) 0.0333(18) 0.0026(13) 0.0099(17) 0.0068(18) C23 0.047(2) 0.0358(16) 0.0310(15) 0.0024(12) 0.0064(18) 0.0042(19) C24 0.042(2) 0.0326(15) 0.0290(15) 0.0021(13) 0.0072(17) 0.006(2) C25 0.044(3) 0.049(2) 0.041(3) -0.012(2) -0.001(2) 0.000(2) C26 0.038(2) 0.036(2) 0.042(3) 0.0017(19) 0.0062(19) 0.0019(19) C19A 0.043(2) 0.028(2) 0.029(2) 0.001(2) 0.007(2) 0.006(2) C20A 0.040(2) 0.027(2) 0.031(2) 0.005(2) 0.008(2) 0.007(2) C21A 0.044(2) 0.029(2) 0.030(2) 0.0010(19) 0.005(2) 0.003(2) C22A 0.040(2) 0.033(2) 0.032(2) 0.000(2) 0.004(2) 0.004(2) C23A 0.043(3) 0.033(2) 0.030(2) -0.0043(19) 0.004(2) 0.001(3) C24A 0.043(2) 0.033(2) 0.031(2) 0.003(2) 0.006(2) 0.003(3) C25A 0.045(4) 0.037(4) 0.026(3) 0.005(3) 0.007(3) 0.002(4) C26A 0.038(4) 0.041(4) 0.043(3) -0.010(3) 0.012(3) -0.004(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 O1 C2 1.2861(18) . ? O1 Li1 1.907(3) . ? O1 Li1 1.950(3) 3_557 ? N1 C4 1.308(2) . ? N1 C6 1.431(2) . ? N1 Li1 2.026(3) . ? C1 C2 1.513(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? Li1 O1 1.950(3) 3_557 ? Li1 O2 1.979(3) . ? Li1 Li1 2.730(5) 3_557 ? O2 C15 1.2603(19) . ? C2 C3 1.378(2) . ? C3 C4 1.432(2) . ? C3 H3 0.9500 . ? C4 C5 1.510(2) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C5 H5D 0.9800 . ? C5 H5E 0.9800 . ? C5 H5F 0.9800 . ? C6 C11 1.397(2) . ? C6 C7 1.407(2) . ? C7 C8 1.394(2) . ? C7 C13 1.500(2) . ? C8 C9 1.380(3) . ? C8 H8 0.9500 . ? C9 C10 1.381(2) . ? C9 H9 0.9500 . ? C10 C11 1.389(2) . ? C10 H10 0.9500 . ? C11 C12 1.506(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.494(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.416(2) . ? C16 C17 1.373(2) . ? C16 H16 0.9500 . ? C18 C17 1.500(2) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C17 N2 1.342(2) . ? N2 C19 1.428(4) . ? N2 C19A 1.460(5) . ? N2 H2 0.95(2) . ? C19 C20 1.390(4) . ? C19 C24 1.407(6) . ? C20 C21 1.398(4) . ? C20 C26 1.499(5) . ? C21 C22 1.384(5) . ? C21 H21A 0.9500 . ? C22 C23 1.385(5) . ? C22 H22A 0.9500 . ? C23 C24 1.391(5) . ? C23 H23A 0.9500 . ? C24 C25 1.515(5) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C19A C24A 1.395(9) . ? C19A C20A 1.4140 . ? C20A C21A 1.3874 . ? C20A C26A 1.503(8) . ? C21A C22A 1.387(8) . ? C21A H21B 0.9500 . ? C22A C23A 1.377(8) . ? C22A H22B 0.9500 . ? C23A C24A 1.409(9) . ? C23A H23B 0.9500 . ? C24A C25A 1.501(9) . ? C25A H25D 0.9800 . ? C25A H25E 0.9800 . ? C25A H25F 0.9800 . ? C26A H26D 0.9800 . ? C26A H26E 0.9800 . ? C26A H26F 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 C2 O1 Li1 124.91(12) . . ? C2 O1 Li1 131.57(12) . 3_557 ? Li1 O1 Li1 90.13(11) . 3_557 ? C4 N1 C6 119.08(13) . . ? C4 N1 Li1 121.56(13) . . ? C6 N1 Li1 119.35(12) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 Li1 O1 89.87(11) . 3_557 ? O1 Li1 O2 129.71(15) . . ? O1 Li1 O2 107.60(13) 3_557 . ? O1 Li1 N1 95.48(12) . . ? O1 Li1 N1 131.94(15) 3_557 . ? O2 Li1 N1 105.09(12) . . ? O1 Li1 Li1 45.57(8) . 3_557 ? O1 Li1 Li1 44.31(8) 3_557 3_557 ? O2 Li1 Li1 131.47(17) . 3_557 ? N1 Li1 Li1 122.95(16) . 3_557 ? C15 O2 Li1 129.11(12) . . ? O1 C2 C3 124.95(14) . . ? O1 C2 C1 115.95(14) . . ? C3 C2 C1 119.04(14) . . ? C2 C3 C4 128.34(14) . . ? C2 C3 H3 115.8 . . ? C4 C3 H3 115.8 . . ? N1 C4 C3 123.45(14) . . ? N1 C4 C5 120.67(14) . . ? C3 C4 C5 115.85(14) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C5 H5D 109.5 . . ? H5A C5 H5D 141.1 . . ? H5B C5 H5D 56.3 . . ? H5C C5 H5D 56.3 . . ? C4 C5 H5E 109.5 . . ? H5A C5 H5E 56.3 . . ? H5B C5 H5E 141.1 . . ? H5C C5 H5E 56.3 . . ? H5D C5 H5E 109.5 . . ? C4 C5 H5F 109.5 . . ? H5A C5 H5F 56.3 . . ? H5B C5 H5F 56.3 . . ? H5C C5 H5F 141.1 . . ? H5D C5 H5F 109.5 . . ? H5E C5 H5F 109.5 . . ? C11 C6 C7 120.33(14) . . ? C11 C6 N1 119.53(13) . . ? C7 C6 N1 120.05(14) . . ? C8 C7 C6 118.42(15) . . ? C8 C7 C13 121.21(14) . . ? C6 C7 C13 120.37(15) . . ? C9 C8 C7 121.52(15) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C10 119.35(16) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C9 C10 C11 121.15(17) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C6 119.21(15) . . ? C10 C11 C12 120.90(15) . . ? C6 C11 C12 119.89(14) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C7 C13 H13A 109.5 . . ? C7 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C7 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C15 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O2 C15 C16 122.25(14) . . ? O2 C15 C14 118.51(14) . . ? C16 C15 C14 119.24(14) . . ? C17 C16 C15 125.06(15) . . ? C17 C16 H16 117.5 . . ? C15 C16 H16 117.5 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C17 C16 121.11(14) . . ? N2 C17 C18 117.88(14) . . ? C16 C17 C18 121.00(14) . . ? C17 N2 C19 125.2(2) . . ? C17 N2 C19A 123.9(3) . . ? C17 N2 H2 114.1(12) . . ? C19 N2 H2 120.0(12) . . ? C19A N2 H2 120.6(12) . . ? C20 C19 C24 122.8(3) . . ? C20 C19 N2 119.3(3) . . ? C24 C19 N2 117.9(3) . . ? C19 C20 C21 117.8(3) . . ? C19 C20 C26 120.0(4) . . ? C21 C20 C26 122.1(4) . . ? C22 C21 C20 120.6(3) . . ? C22 C21 H21A 119.7 . . ? C20 C21 H21A 119.7 . . ? C21 C22 C23 120.3(4) . . ? C21 C22 H22A 119.9 . . ? C23 C22 H22A 119.9 . . ? C22 C23 C24 121.3(4) . . ? C22 C23 H23A 119.3 . . ? C24 C23 H23A 119.3 . . ? C23 C24 C19 117.2(4) . . ? C23 C24 C25 120.0(4) . . ? C19 C24 C25 122.9(4) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C20 C26 H26A 109.5 . . ? C20 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C20 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24A C19A C20A 121.7(4) . . ? C24A C19A N2 123.6(5) . . ? C20A C19A N2 114.2(2) . . ? C21A C20A C19A 118.5 . . ? C21A C20A C26A 120.2(7) . . ? C19A C20A C26A 121.3(7) . . ? C22A C21A C20A 119.6(4) . . ? C22A C21A H21B 120.2 . . ? C20A C21A H21B 120.2 . . ? C23A C22A C21A 122.1(7) . . ? C23A C22A H22B 119.0 . . ? C21A C22A H22B 119.0 . . ? C22A C23A C24A 119.7(7) . . ? C22A C23A H23B 120.2 . . ? C24A C23A H23B 120.2 . . ? C19A C24A C23A 118.1(7) . . ? C19A C24A C25A 119.7(8) . . ? C23A C24A C25A 122.2(8) . . ? C24A C25A H25D 109.5 . . ? C24A C25A H25E 109.5 . . ? H25D C25A H25E 109.5 . . ? C24A C25A H25F 109.5 . . ? H25D C25A H25F 109.5 . . ? H25E C25A H25F 109.5 . . ? C20A C26A H26D 109.5 . . ? C20A C26A H26E 109.5 . . ? H26D C26A H26E 109.5 . . ? C20A C26A H26F 109.5 . . ? H26D C26A H26F 109.5 . . ? H26E C26A H26F 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 C2 O1 Li1 O1 144.16(14) . . . 3_557 ? Li1 O1 Li1 O1 0.0 3_557 . . 3_557 ? C2 O1 Li1 O2 -102.81(19) . . . . ? Li1 O1 Li1 O2 113.0(2) 3_557 . . . ? C2 O1 Li1 N1 11.99(18) . . . . ? Li1 O1 Li1 N1 -132.16(15) 3_557 . . . ? C2 O1 Li1 Li1 144.15(14) . . . 3_557 ? C4 N1 Li1 O1 -8.46(18) . . . . ? C6 N1 Li1 O1 172.73(11) . . . . ? C4 N1 Li1 O1 -103.2(2) . . . 3_557 ? C6 N1 Li1 O1 78.0(2) . . . 3_557 ? C4 N1 Li1 O2 125.22(14) . . . . ? C6 N1 Li1 O2 -53.60(17) . . . . ? C4 N1 Li1 Li1 -47.6(3) . . . 3_557 ? C6 N1 Li1 Li1 133.62(18) . . . 3_557 ? O1 Li1 O2 C15 -61.5(2) . . . . ? O1 Li1 O2 C15 43.5(2) 3_557 . . . ? N1 Li1 O2 C15 -172.18(13) . . . . ? Li1 Li1 O2 C15 -0.3(3) 3_557 . . . ? Li1 O1 C2 C3 -8.2(2) . . . . ? Li1 O1 C2 C3 120.27(18) 3_557 . . . ? Li1 O1 C2 C1 174.68(14) . . . . ? Li1 O1 C2 C1 -56.8(2) 3_557 . . . ? O1 C2 C3 C4 -3.3(3) . . . . ? C1 C2 C3 C4 173.69(16) . . . . ? C6 N1 C4 C3 -179.90(14) . . . . ? Li1 N1 C4 C3 1.3(2) . . . . ? C6 N1 C4 C5 -2.1(2) . . . . ? Li1 N1 C4 C5 179.13(15) . . . . ? C2 C3 C4 N1 6.9(3) . . . . ? C2 C3 C4 C5 -171.10(17) . . . . ? C4 N1 C6 C11 98.14(17) . . . . ? Li1 N1 C6 C11 -83.02(17) . . . . ? C4 N1 C6 C7 -85.10(18) . . . . ? Li1 N1 C6 C7 93.74(17) . . . . ? C11 C6 C7 C8 -1.6(2) . . . . ? N1 C6 C7 C8 -178.34(13) . . . . ? C11 C6 C7 C13 178.85(14) . . . . ? N1 C6 C7 C13 2.1(2) . . . . ? C6 C7 C8 C9 1.0(2) . . . . ? C13 C7 C8 C9 -179.46(15) . . . . ? C7 C8 C9 C10 0.3(2) . . . . ? C8 C9 C10 C11 -1.1(2) . . . . ? C9 C10 C11 C6 0.5(2) . . . . ? C9 C10 C11 C12 -179.51(15) . . . . ? C7 C6 C11 C10 0.9(2) . . . . ? N1 C6 C11 C10 177.64(13) . . . . ? C7 C6 C11 C12 -179.12(14) . . . . ? N1 C6 C11 C12 -2.4(2) . . . . ? Li1 O2 C15 C16 -153.22(15) . . . . ? Li1 O2 C15 C14 27.3(2) . . . . ? O2 C15 C16 C17 -2.9(3) . . . . ? C14 C15 C16 C17 176.54(15) . . . . ? C15 C16 C17 N2 -0.9(3) . . . . ? C15 C16 C17 C18 178.81(16) . . . . ? C16 C17 N2 C19 176.8(2) . . . . ? C18 C17 N2 C19 -2.8(3) . . . . ? C16 C17 N2 C19A 172.9(3) . . . . ? C18 C17 N2 C19A -6.7(3) . . . . ? C17 N2 C19 C20 -96.8(3) . . . . ? C19A N2 C19 C20 -28(8) . . . . ? C17 N2 C19 C24 82.5(6) . . . . ? C19A N2 C19 C24 151(8) . . . . ? C24 C19 C20 C21 -0.3(7) . . . . ? N2 C19 C20 C21 179.0(3) . . . . ? C24 C19 C20 C26 177.5(9) . . . . ? N2 C19 C20 C26 -3.3(5) . . . . ? C19 C20 C21 C22 0.0(5) . . . . ? C26 C20 C21 C22 -177.7(7) . . . . ? C20 C21 C22 C23 0.6(6) . . . . ? C21 C22 C23 C24 -1.0(9) . . . . ? C22 C23 C24 C19 0.7(11) . . . . ? C22 C23 C24 C25 -180.0(8) . . . . ? C20 C19 C24 C23 -0.1(10) . . . . ? N2 C19 C24 C23 -179.4(6) . . . . ? C20 C19 C24 C25 -179.4(7) . . . . ? N2 C19 C24 C25 1.4(12) . . . . ? C17 N2 C19A C24A 88.9(11) . . . . ? C19 N2 C19A C24A -24(7) . . . . ? C17 N2 C19A C20A -99.5(2) . . . . ? C19 N2 C19A C20A 147(8) . . . . ? C24A C19A C20A C21A -6.4(10) . . . . ? N2 C19A C20A C21A -178.1(3) . . . . ? C24A C19A C20A C26A 174.3(17) . . . . ? N2 C19A C20A C26A 2.5(8) . . . . ? C19A C20A C21A C22A 2.2(6) . . . . ? C26A C20A C21A C22A -178.4(14) . . . . ? C20A C21A C22A C23A 1.4(11) . . . . ? C21A C22A C23A C24A -1.1(17) . . . . ? C20A C19A C24A C23A 6.6(19) . . . . ? N2 C19A C24A C23A 177.6(10) . . . . ? C20A C19A C24A C25A -173.9(11) . . . . ? N2 C19A C24A C25A -3(2) . . . . ? C22A C23A C24A C19A -3(2) . . . . ? C22A C23A C24A C25A 177.7(14) . . . . ? 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 N2 H2 O2 0.95(2) 1.90(2) 2.6678(18) 136.2(17) . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 59.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.232 _refine_diff_density_min -0.156 _refine_diff_density_rms 0.035 # Attachment 'structure2.cif' data_mooimm _database_code_depnum_ccdc_archive 'CCDC 720402' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H32 Mo N2 O4' _chemical_formula_sum 'C26 H32 Mo N2 O4' _chemical_formula_weight 532.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo Mo -1.6832 0.6857 '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' 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' _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 11.762(5) _cell_length_b 14.486(5) _cell_length_c 15.238(5) _cell_angle_alpha 90.00 _cell_angle_beta 101.198(5) _cell_angle_gamma 90.00 _cell_volume 2546.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9404 _cell_measurement_theta_min 3.13 _cell_measurement_theta_max 30.02 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.548 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7212 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_decay_% ? _diffrn_reflns_number 126854 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0129 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.45 _diffrn_reflns_theta_max 30.02 _reflns_number_total 7401 _reflns_number_gt 6959 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-92 (Giacovazzo, 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0173P)^2^+1.7643P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7401 _refine_ls_number_parameters 306 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0218 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0506 _refine_ls_wR_factor_gt 0.0495 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 Mo1 Mo 0.249517(7) 0.196042(6) 0.825815(6) 0.01014(3) Uani 1 1 d . . . O1 O 0.15505(7) 0.28427(6) 0.79122(6) 0.01754(16) Uani 1 1 d . . . O2 O 0.32959(7) 0.19020(6) 0.74320(6) 0.01717(16) Uani 1 1 d . . . O3 O 0.32714(7) 0.07308(5) 0.88269(5) 0.01437(15) Uani 1 1 d . . . O4 O 0.19239(7) 0.19000(6) 0.94810(6) 0.01633(16) Uani 1 1 d . . . N1 N 0.11232(8) 0.09969(7) 0.77407(6) 0.01340(17) Uani 1 1 d . . . N2 N 0.38671(8) 0.27084(6) 0.90904(6) 0.01206(17) Uani 1 1 d . . . C1 C 0.35880(13) -0.05721(10) 0.97866(11) 0.0309(3) Uani 1 1 d . . . H1A H 0.4263 -0.0775 0.9548 0.046 Uiso 1 1 calc R . . H1B H 0.3160 -0.1113 0.9932 0.046 Uiso 1 1 calc R . . H1C H 0.3847 -0.0204 1.0328 0.046 Uiso 1 1 calc R . . C2 C 0.28125(11) 0.00036(8) 0.90982(8) 0.0177(2) Uani 1 1 d . . . C3 C 0.16880(11) -0.02682(8) 0.87654(9) 0.0206(2) Uani 1 1 d . . . H3 H 0.1399 -0.0786 0.9036 0.025 Uiso 1 1 calc R . . C4 C 0.09367(10) 0.01682(8) 0.80520(8) 0.0171(2) Uani 1 1 d . . . C5 C -0.01197(11) -0.03738(9) 0.76171(10) 0.0256(3) Uani 1 1 d . . . H5A H -0.0820 -0.0021 0.7653 0.038 Uiso 1 1 calc R . . H5B H -0.0136 -0.0965 0.7928 0.038 Uiso 1 1 calc R . . H5C H -0.0089 -0.0488 0.6988 0.038 Uiso 1 1 calc R . . C6 C 0.03190(10) 0.13209(8) 0.69607(8) 0.0173(2) Uani 1 1 d . . . C7 C -0.06584(11) 0.18254(9) 0.70801(10) 0.0251(3) Uani 1 1 d . . . C8 C -0.14016(13) 0.21516(11) 0.63171(13) 0.0382(4) Uani 1 1 d . . . H8 H -0.2072 0.2491 0.6379 0.046 Uiso 1 1 calc R . . C9 C -0.11818(16) 0.19905(12) 0.54755(13) 0.0453(5) Uani 1 1 d . . . H9 H -0.1696 0.2223 0.4965 0.054 Uiso 1 1 calc R . . C10 C -0.02164(15) 0.14920(12) 0.53711(10) 0.0383(4) Uani 1 1 d . . . H10 H -0.0073 0.1385 0.4787 0.046 Uiso 1 1 calc R . . C11 C 0.05559(12) 0.11420(10) 0.61145(9) 0.0242(3) Uani 1 1 d . . . C12 C 0.16011(13) 0.05938(12) 0.59999(10) 0.0331(3) Uani 1 1 d . . . H12A H 0.2295 0.0981 0.6149 0.050 Uiso 1 1 calc R . . H12B H 0.1507 0.0386 0.5378 0.050 Uiso 1 1 calc R . . H12C H 0.1684 0.0056 0.6398 0.050 Uiso 1 1 calc R . . C13 C -0.09128(12) 0.20049(11) 0.79951(12) 0.0350(3) Uani 1 1 d . . . H13A H -0.1447 0.2528 0.7966 0.052 Uiso 1 1 calc R . . H13B H -0.0189 0.2148 0.8412 0.052 Uiso 1 1 calc R . . H13C H -0.1268 0.1455 0.8203 0.052 Uiso 1 1 calc R . . C14 C 0.18843(13) 0.14042(10) 1.09522(9) 0.0269(3) Uani 1 1 d . . . H14A H 0.1247 0.1814 1.1029 0.040 Uiso 1 1 calc R . . H14B H 0.2421 0.1332 1.1526 0.040 Uiso 1 1 calc R . . H14C H 0.1572 0.0799 1.0741 0.040 Uiso 1 1 calc R . . C15 C 0.25158(11) 0.18134(8) 1.02801(8) 0.0176(2) Uani 1 1 d . . . C16 C 0.36519(11) 0.21085(8) 1.05298(8) 0.0191(2) Uani 1 1 d . . . H16 H 0.4064 0.1952 1.1110 0.023 Uiso 1 1 calc R . . C17 C 0.42301(10) 0.26290(8) 0.99701(8) 0.0156(2) Uani 1 1 d . . . C18 C 0.53013(12) 0.31461(10) 1.04156(9) 0.0244(3) Uani 1 1 d . . . H18A H 0.5913 0.3065 1.0067 0.037 Uiso 1 1 calc R . . H18B H 0.5568 0.2905 1.1022 0.037 Uiso 1 1 calc R . . H18C H 0.5119 0.3804 1.0447 0.037 Uiso 1 1 calc R . . C19 C 0.43995(9) 0.33967(7) 0.86129(7) 0.01317(19) Uani 1 1 d . . . C20 C 0.39242(10) 0.42871(8) 0.85376(8) 0.0172(2) Uani 1 1 d . . . C21 C 0.43761(13) 0.49313(9) 0.80172(9) 0.0252(3) Uani 1 1 d . . . H21 H 0.4051 0.5533 0.7945 0.030 Uiso 1 1 calc R . . C22 C 0.52901(14) 0.47101(10) 0.76041(10) 0.0296(3) Uani 1 1 d . . . H22 H 0.5590 0.5158 0.7254 0.035 Uiso 1 1 calc R . . C23 C 0.57644(12) 0.38322(10) 0.77050(9) 0.0244(3) Uani 1 1 d . . . H23 H 0.6400 0.3686 0.7429 0.029 Uiso 1 1 calc R . . C24 C 0.53265(10) 0.31575(8) 0.82034(8) 0.0167(2) Uani 1 1 d . . . C25 C 0.58602(11) 0.22109(9) 0.83061(9) 0.0221(2) Uani 1 1 d . . . H25A H 0.6158 0.2055 0.7767 0.033 Uiso 1 1 calc R . . H25B H 0.5273 0.1758 0.8392 0.033 Uiso 1 1 calc R . . H25C H 0.6498 0.2203 0.8826 0.033 Uiso 1 1 calc R . . C26 C 0.29750(11) 0.45545(9) 0.90231(9) 0.0223(2) Uani 1 1 d . . . H26A H 0.3280 0.4558 0.9669 0.033 Uiso 1 1 calc R . . H26B H 0.2339 0.4108 0.8886 0.033 Uiso 1 1 calc R . . H26C H 0.2688 0.5172 0.8831 0.033 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 0.01089(4) 0.00996(4) 0.00949(5) 0.00033(3) 0.00174(3) -0.00139(3) O1 0.0174(4) 0.0149(4) 0.0182(4) 0.0027(3) -0.0018(3) -0.0004(3) O2 0.0175(4) 0.0183(4) 0.0158(4) -0.0001(3) 0.0035(3) -0.0057(3) O3 0.0153(4) 0.0115(3) 0.0164(4) 0.0010(3) 0.0033(3) 0.0000(3) O4 0.0184(4) 0.0177(4) 0.0144(4) -0.0003(3) 0.0068(3) -0.0004(3) N1 0.0119(4) 0.0151(4) 0.0131(4) -0.0005(3) 0.0022(3) -0.0021(3) N2 0.0134(4) 0.0115(4) 0.0112(4) 0.0004(3) 0.0020(3) -0.0013(3) C1 0.0314(7) 0.0201(6) 0.0363(8) 0.0133(6) -0.0056(6) -0.0011(5) C2 0.0228(5) 0.0129(5) 0.0173(5) 0.0027(4) 0.0034(4) 0.0004(4) C3 0.0238(6) 0.0150(5) 0.0228(6) 0.0050(4) 0.0039(5) -0.0050(4) C4 0.0168(5) 0.0166(5) 0.0184(5) -0.0013(4) 0.0050(4) -0.0052(4) C5 0.0232(6) 0.0232(6) 0.0290(7) 0.0012(5) 0.0015(5) -0.0130(5) C6 0.0150(5) 0.0171(5) 0.0178(5) 0.0011(4) -0.0019(4) -0.0052(4) C7 0.0145(5) 0.0225(6) 0.0351(7) -0.0006(5) -0.0033(5) -0.0031(4) C8 0.0215(6) 0.0272(7) 0.0565(11) 0.0065(7) -0.0157(7) -0.0029(5) C9 0.0411(9) 0.0377(9) 0.0432(10) 0.0154(7) -0.0260(8) -0.0130(7) C10 0.0468(9) 0.0430(9) 0.0184(7) 0.0048(6) -0.0102(6) -0.0206(7) C11 0.0274(6) 0.0268(6) 0.0165(6) -0.0014(5) -0.0007(5) -0.0122(5) C12 0.0355(7) 0.0440(9) 0.0223(7) -0.0149(6) 0.0117(6) -0.0114(6) C13 0.0171(6) 0.0384(8) 0.0512(10) -0.0093(7) 0.0111(6) 0.0020(5) C14 0.0387(7) 0.0280(7) 0.0180(6) 0.0017(5) 0.0152(5) -0.0049(6) C15 0.0276(6) 0.0141(5) 0.0135(5) -0.0003(4) 0.0097(4) 0.0007(4) C16 0.0263(6) 0.0201(5) 0.0105(5) 0.0017(4) 0.0027(4) 0.0006(4) C17 0.0171(5) 0.0158(5) 0.0128(5) -0.0017(4) 0.0002(4) 0.0008(4) C18 0.0237(6) 0.0300(7) 0.0163(6) -0.0035(5) -0.0040(5) -0.0062(5) C19 0.0144(5) 0.0127(5) 0.0120(5) -0.0010(4) 0.0015(4) -0.0044(4) C20 0.0225(5) 0.0122(5) 0.0169(5) -0.0021(4) 0.0036(4) -0.0028(4) C21 0.0402(7) 0.0121(5) 0.0241(6) 0.0000(4) 0.0081(5) -0.0055(5) C22 0.0431(8) 0.0214(6) 0.0274(7) 0.0002(5) 0.0147(6) -0.0151(6) C23 0.0245(6) 0.0276(6) 0.0238(6) -0.0043(5) 0.0118(5) -0.0114(5) C24 0.0150(5) 0.0185(5) 0.0166(5) -0.0031(4) 0.0031(4) -0.0046(4) C25 0.0171(5) 0.0242(6) 0.0255(6) -0.0016(5) 0.0056(5) 0.0029(4) C26 0.0256(6) 0.0152(5) 0.0267(6) -0.0037(5) 0.0067(5) 0.0024(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 O1 1.7083(9) . ? Mo1 O2 1.7144(10) . ? Mo1 O4 2.1018(10) . ? Mo1 O3 2.1095(10) . ? Mo1 N2 2.1427(11) . ? Mo1 N1 2.1632(11) . ? O3 C2 1.2879(14) . ? O4 C15 1.2861(15) . ? N1 C4 1.3246(15) . ? N1 C6 1.4461(15) . ? N2 C17 1.3304(15) . ? N2 C19 1.4466(14) . ? C1 C2 1.5021(17) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.3787(18) . ? C3 C4 1.4104(17) . ? C3 H3 0.9500 . ? C4 C5 1.5099(17) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C11 1.3953(18) . ? C6 C7 1.4036(18) . ? C7 C8 1.394(2) . ? C7 C13 1.504(2) . ? C8 C9 1.376(3) . ? C8 H8 0.9500 . ? C9 C10 1.381(3) . ? C9 H9 0.9500 . ? C10 C11 1.402(2) . ? C10 H10 0.9500 . ? C11 C12 1.502(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.4991(17) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.3841(19) . ? C16 C17 1.4084(17) . ? C16 H16 0.9500 . ? C17 C18 1.5092(17) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.4009(16) . ? C19 C20 1.4016(16) . ? C20 C21 1.3949(17) . ? C20 C26 1.5049(18) . ? C21 C22 1.385(2) . ? C21 H21 0.9500 . ? C22 C23 1.385(2) . ? C22 H22 0.9500 . ? C23 C24 1.3962(17) . ? C23 H23 0.9500 . ? C24 C25 1.5035(18) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 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 O1 Mo1 O2 103.15(5) . . ? O1 Mo1 O4 90.23(4) . . ? O2 Mo1 O4 164.73(4) . . ? O1 Mo1 O3 164.18(4) . . ? O2 Mo1 O3 90.25(4) . . ? O4 Mo1 O3 77.76(3) . . ? O1 Mo1 N2 100.04(5) . . ? O2 Mo1 N2 90.09(5) . . ? O4 Mo1 N2 80.21(4) . . ? O3 Mo1 N2 88.15(4) . . ? O1 Mo1 N1 88.61(5) . . ? O2 Mo1 N1 100.24(4) . . ? O4 Mo1 N1 87.25(4) . . ? O3 Mo1 N1 80.65(4) . . ? N2 Mo1 N1 164.73(4) . . ? C2 O3 Mo1 130.36(8) . . ? C15 O4 Mo1 129.50(8) . . ? C4 N1 C6 117.46(10) . . ? C4 N1 Mo1 128.17(8) . . ? C6 N1 Mo1 114.38(7) . . ? C17 N2 C19 118.74(9) . . ? C17 N2 Mo1 127.59(8) . . ? C19 N2 Mo1 113.62(7) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O3 C2 C3 123.19(11) . . ? O3 C2 C1 116.28(11) . . ? C3 C2 C1 120.49(11) . . ? C2 C3 C4 124.63(11) . . ? C2 C3 H3 117.7 . . ? C4 C3 H3 117.7 . . ? N1 C4 C3 124.03(11) . . ? N1 C4 C5 119.58(11) . . ? C3 C4 C5 116.37(11) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 122.14(12) . . ? C11 C6 N1 118.89(11) . . ? C7 C6 N1 118.94(11) . . ? C8 C7 C6 117.71(15) . . ? C8 C7 C13 120.59(14) . . ? C6 C7 C13 121.70(12) . . ? C9 C8 C7 121.24(16) . . ? C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C10 120.23(14) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C11 120.95(16) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C6 C11 C10 117.73(14) . . ? C6 C11 C12 121.37(12) . . ? C10 C11 C12 120.91(14) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C7 C13 H13A 109.5 . . ? C7 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C7 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 H14A 109.5 . . ? C15 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C15 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O4 C15 C16 123.11(11) . . ? O4 C15 C14 115.88(12) . . ? C16 C15 C14 120.96(12) . . ? C15 C16 C17 123.56(11) . . ? C15 C16 H16 118.2 . . ? C17 C16 H16 118.2 . . ? N2 C17 C16 123.93(11) . . ? N2 C17 C18 119.14(11) . . ? C16 C17 C18 116.90(11) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 121.58(10) . . ? C24 C19 N2 120.26(10) . . ? C20 C19 N2 118.08(10) . . ? C21 C20 C19 118.18(11) . . ? C21 C20 C26 120.55(11) . . ? C19 C20 C26 121.26(11) . . ? C22 C21 C20 121.25(12) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 119.57(12) . . ? C21 C22 H22 120.2 . . ? C23 C22 H22 120.2 . . ? C22 C23 C24 121.33(12) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C23 C24 C19 118.06(11) . . ? C23 C24 C25 120.29(11) . . ? C19 C24 C25 121.64(11) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C20 C26 H26A 109.5 . . ? C20 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C20 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 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 O1 Mo1 O3 C2 15.49(19) . . . . ? O2 Mo1 O3 C2 -132.70(10) . . . . ? O4 Mo1 O3 C2 56.83(10) . . . . ? N2 Mo1 O3 C2 137.21(10) . . . . ? N1 Mo1 O3 C2 -32.37(10) . . . . ? O1 Mo1 O4 C15 -136.83(10) . . . . ? O2 Mo1 O4 C15 14.58(19) . . . . ? O3 Mo1 O4 C15 53.55(10) . . . . ? N2 Mo1 O4 C15 -36.68(10) . . . . ? N1 Mo1 O4 C15 134.58(10) . . . . ? O1 Mo1 N1 C4 -147.16(10) . . . . ? O2 Mo1 N1 C4 109.73(10) . . . . ? O4 Mo1 N1 C4 -56.87(10) . . . . ? O3 Mo1 N1 C4 21.18(10) . . . . ? N2 Mo1 N1 C4 -22.2(2) . . . . ? O1 Mo1 N1 C6 32.39(8) . . . . ? O2 Mo1 N1 C6 -70.72(8) . . . . ? O4 Mo1 N1 C6 122.69(8) . . . . ? O3 Mo1 N1 C6 -159.27(8) . . . . ? N2 Mo1 N1 C6 157.38(12) . . . . ? O1 Mo1 N2 C17 115.14(10) . . . . ? O2 Mo1 N2 C17 -141.49(10) . . . . ? O4 Mo1 N2 C17 26.65(9) . . . . ? O3 Mo1 N2 C17 -51.25(10) . . . . ? N1 Mo1 N2 C17 -8.58(19) . . . . ? O1 Mo1 N2 C19 -62.15(8) . . . . ? O2 Mo1 N2 C19 41.22(8) . . . . ? O4 Mo1 N2 C19 -150.63(8) . . . . ? O3 Mo1 N2 C19 131.47(7) . . . . ? N1 Mo1 N2 C19 174.14(11) . . . . ? Mo1 O3 C2 C3 26.19(18) . . . . ? Mo1 O3 C2 C1 -156.10(10) . . . . ? O3 C2 C3 C4 4.9(2) . . . . ? C1 C2 C3 C4 -172.76(13) . . . . ? C6 N1 C4 C3 175.29(11) . . . . ? Mo1 N1 C4 C3 -5.17(17) . . . . ? C6 N1 C4 C5 -2.98(16) . . . . ? Mo1 N1 C4 C5 176.56(9) . . . . ? C2 C3 C4 N1 -15.0(2) . . . . ? C2 C3 C4 C5 163.36(13) . . . . ? C4 N1 C6 C11 -91.22(14) . . . . ? Mo1 N1 C6 C11 89.18(12) . . . . ? C4 N1 C6 C7 90.41(14) . . . . ? Mo1 N1 C6 C7 -89.20(11) . . . . ? C11 C6 C7 C8 -0.10(19) . . . . ? N1 C6 C7 C8 178.22(11) . . . . ? C11 C6 C7 C13 179.29(12) . . . . ? N1 C6 C7 C13 -2.39(18) . . . . ? C6 C7 C8 C9 -0.4(2) . . . . ? C13 C7 C8 C9 -179.82(14) . . . . ? C7 C8 C9 C10 0.5(2) . . . . ? C8 C9 C10 C11 0.0(2) . . . . ? C7 C6 C11 C10 0.53(19) . . . . ? N1 C6 C11 C10 -177.79(11) . . . . ? C7 C6 C11 C12 -179.47(12) . . . . ? N1 C6 C11 C12 2.21(18) . . . . ? C9 C10 C11 C6 -0.5(2) . . . . ? C9 C10 C11 C12 179.54(14) . . . . ? Mo1 O4 C15 C16 27.28(17) . . . . ? Mo1 O4 C15 C14 -155.27(9) . . . . ? O4 C15 C16 C17 7.85(19) . . . . ? C14 C15 C16 C17 -169.48(12) . . . . ? C19 N2 C17 C16 168.25(11) . . . . ? Mo1 N2 C17 C16 -8.91(17) . . . . ? C19 N2 C17 C18 -9.63(16) . . . . ? Mo1 N2 C17 C18 173.21(8) . . . . ? C15 C16 C17 N2 -16.59(19) . . . . ? C15 C16 C17 C18 161.34(12) . . . . ? C17 N2 C19 C24 94.54(13) . . . . ? Mo1 N2 C19 C24 -87.92(11) . . . . ? C17 N2 C19 C20 -88.55(13) . . . . ? Mo1 N2 C19 C20 88.99(11) . . . . ? C24 C19 C20 C21 1.93(17) . . . . ? N2 C19 C20 C21 -174.94(11) . . . . ? C24 C19 C20 C26 -176.40(11) . . . . ? N2 C19 C20 C26 6.74(16) . . . . ? C19 C20 C21 C22 -1.7(2) . . . . ? C26 C20 C21 C22 176.60(13) . . . . ? C20 C21 C22 C23 0.2(2) . . . . ? C21 C22 C23 C24 1.1(2) . . . . ? C22 C23 C24 C19 -0.93(19) . . . . ? C22 C23 C24 C25 -179.73(13) . . . . ? C20 C19 C24 C23 -0.62(17) . . . . ? N2 C19 C24 C23 176.17(10) . . . . ? C20 C19 C24 C25 178.16(11) . . . . ? N2 C19 C24 C25 -5.04(17) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.02 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.470 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.052