# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_address ; Department of Chemistry Texas A&M University, College Station, TX United States of America ; ; Department of Chemistry Texas A&M University, College Station, TX United States of America ; ; Department of Chemistry Texas A&M University, College Station, TX United States of America ; #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author ; Kim R. Dunbar Department of Chemistry Texas A&M University, College Station, TX United States of America ; _publ_contact_author_email dunbar@mail.chem.tamu.edu _publ_contact_author_fax (979)845-7177 _publ_contact_author_phone (979)845-5235 _publ_contact_letter ; ; _publ_requested_category 'Coordination Chemistry' _publ_requested_coeditor_name ? _publ_author_name K.Dunbar _publ_contact_author_name 'Kim R. Dunbar' data_Co3Mo2TBP _database_code_depnum_ccdc_archive 'CCDC 723434' #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C119 H136 Co3 Mo2 N26 O10' _chemical_formula_weight 2459.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.387(2) _cell_length_b 25.463(3) _cell_length_c 24.634(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.205(2) _cell_angle_gamma 90.00 _cell_volume 12036(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 59294 _cell_measurement_theta_min 2.2502 _cell_measurement_theta_max 22.3088 _exptl_crystal_description column _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.357 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5108 _exptl_absorpt_coefficient_mu 0.675 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8547 _exptl_absorpt_correction_T_max 0.9355 _exptl_absorpt_process_details 'SADABS: Bruker,2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'BRUKER APEX' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 89907 _diffrn_reflns_av_R_equivalents 0.0445 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 22.41 _reflns_number_total 15460 _reflns_number_gt 11451 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diomand _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1229P)^2^+43.4346P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15460 _refine_ls_number_parameters 1461 _refine_ls_number_restraints 83 _refine_ls_R_factor_all 0.0956 _refine_ls_R_factor_gt 0.0663 _refine_ls_wR_factor_ref 0.2132 _refine_ls_wR_factor_gt 0.1793 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.092 _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 0.32430(3) 0.34252(3) 0.12938(3) 0.0427(2) Uani 1 1 d . . . Mo2 Mo 0.14174(4) 0.51780(3) 0.25621(3) 0.0470(2) Uani 1 1 d . . . Co1 Co 0.36371(5) 0.54235(4) 0.16167(4) 0.0362(3) Uani 1 1 d . . . Co2 Co 0.05681(5) 0.37076(4) 0.11370(4) 0.0366(3) Uani 1 1 d . . . Co3 Co 0.29616(5) 0.36227(4) 0.33516(4) 0.0403(3) Uani 1 1 d . . . N1 N 0.3350(3) 0.4704(3) 0.1300(3) 0.0497(17) Uani 1 1 d . . . N2 N 0.1547(4) 0.3429(3) 0.1247(2) 0.0508(17) Uani 1 1 d . . . N3 N 0.3253(3) 0.3606(2) 0.2606(3) 0.0558(18) Uani 1 1 d . . . N4 N 0.3097(5) 0.3192(4) -0.0029(4) 0.090(3) Uani 1 1 d . . . N5 N 0.4957(4) 0.3420(4) 0.1386(3) 0.079(2) Uani 1 1 d . . . N6 N 0.3107(4) 0.2153(3) 0.1496(4) 0.082(3) Uani 1 1 d . . . N7 N 0.2872(4) 0.5383(2) 0.2078(3) 0.0535(17) Uani 1 1 d . . . N8 N 0.0935(3) 0.4368(3) 0.1547(3) 0.0473(16) Uani 1 1 d . . . N9 N 0.2225(4) 0.4156(3) 0.3120(3) 0.0551(18) Uani 1 1 d . . . N10 N 0.0914(4) 0.6268(3) 0.1911(3) 0.066(2) Uani 1 1 d . . . N11 N 0.1986(5) 0.5825(4) 0.3684(4) 0.096(3) Uani 1 1 d . . . N12 N -0.0148(5) 0.4934(5) 0.2881(5) 0.116(4) Uani 1 1 d . . . N13 N 0.3060(3) 0.5899(2) 0.0992(2) 0.0410(14) Uani 1 1 d . . . N14 N 0.4339(3) 0.5501(2) 0.1058(3) 0.0451(15) Uani 1 1 d . . . N15 N 0.4082(3) 0.6104(2) 0.1995(2) 0.0415(15) Uani 1 1 d . . . N16 N 0.4436(3) 0.5117(2) 0.2236(2) 0.0405(14) Uani 1 1 d . . . N17 N 0.0087(3) 0.2994(2) 0.0873(2) 0.0404(14) Uani 1 1 d . . . N18 N 0.0273(3) 0.3390(2) 0.1877(2) 0.0404(14) Uani 1 1 d . . . N19 N 0.0678(3) 0.3947(2) 0.0315(2) 0.0400(14) Uani 1 1 d . . . N20 N -0.0387(3) 0.4072(2) 0.0876(3) 0.0446(15) Uani 1 1 d . . . N21 N 0.2255(3) 0.2978(2) 0.3137(3) 0.0462(16) Uani 1 1 d . . . N22 N 0.2584(3) 0.3489(2) 0.4085(3) 0.0491(16) Uani 1 1 d . . . N23 N 0.3808(4) 0.3184(3) 0.3667(3) 0.0587(18) Uani 1 1 d . . . N24 N 0.3703(3) 0.4215(2) 0.3654(2) 0.0434(15) Uani 1 1 d . . . C1 C 0.3269(3) 0.4268(3) 0.1232(3) 0.0315(15) Uani 1 1 d . . . C2 C 0.2136(4) 0.3422(3) 0.1265(3) 0.0326(15) Uani 1 1 d . . . C3 C 0.3310(3) 0.3549(3) 0.2159(3) 0.0301(15) Uani 1 1 d . . . C4 C 0.3143(4) 0.3292(4) 0.0430(4) 0.062(2) Uani 1 1 d . . . C5 C 0.4371(5) 0.3423(3) 0.1351(3) 0.053(2) Uani 1 1 d . . . C6 C 0.3189(4) 0.2591(4) 0.1428(4) 0.056(2) Uani 1 1 d . . . C7 C 0.2393(4) 0.5316(3) 0.2273(3) 0.0344(16) Uani 1 1 d . . . C8 C 0.1115(3) 0.4679(3) 0.1861(3) 0.0317(15) Uani 1 1 d . . . C9 C 0.1876(3) 0.4493(3) 0.2951(3) 0.0314(15) Uani 1 1 d . . . C10 C 0.1072(4) 0.5888(3) 0.2139(3) 0.052(2) Uani 1 1 d . . . C11 C 0.1776(5) 0.5611(4) 0.3289(4) 0.065(2) Uani 1 1 d . . . C12 C 0.0407(5) 0.5026(4) 0.2775(4) 0.078(3) Uani 1 1 d . . . C13 C 0.2443(4) 0.6112(3) 0.0991(3) 0.0431(18) Uani 1 1 d . . . H13A H 0.2198 0.6030 0.1288 0.052 Uiso 1 1 calc R . . C14 C 0.2121(4) 0.6452(3) 0.0584(3) 0.052(2) Uani 1 1 d . . . C15 C 0.2470(5) 0.6559(3) 0.0141(4) 0.062(2) Uani 1 1 d . . . C16 C 0.3137(5) 0.6328(3) 0.0138(3) 0.057(2) Uani 1 1 d . . . C17 C 0.3552(6) 0.6405(4) -0.0294(4) 0.072(3) Uani 1 1 d . . . H17A H 0.3376 0.6614 -0.0602 0.087 Uiso 1 1 calc R . . C18 C 0.4186(7) 0.6186(4) -0.0270(4) 0.074(3) Uani 1 1 d . . . H18A H 0.4441 0.6245 -0.0566 0.089 Uiso 1 1 calc R . . C19 C 0.4497(5) 0.5869(3) 0.0181(4) 0.061(2) Uani 1 1 d . . . C20 C 0.5181(5) 0.5647(4) 0.0244(4) 0.068(3) Uani 1 1 d . . . C21 C 0.5418(5) 0.5385(4) 0.0713(5) 0.068(3) Uani 1 1 d . . . C22 C 0.4982(4) 0.5314(3) 0.1099(4) 0.053(2) Uani 1 1 d . . . H22A H 0.5153 0.5116 0.1417 0.063 Uiso 1 1 calc R . . C23 C 0.3414(4) 0.6013(3) 0.0577(3) 0.0450(19) Uani 1 1 d . . . C24 C 0.4107(4) 0.5785(3) 0.0602(3) 0.0465(19) Uani 1 1 d . . . C25 C 0.1426(5) 0.6684(4) 0.0646(4) 0.073(3) Uani 1 1 d . . . H25A H 0.1271 0.6914 0.0333 0.109 Uiso 1 1 calc R . . H25B H 0.1467 0.6889 0.0986 0.109 Uiso 1 1 calc R . . H25C H 0.1086 0.6402 0.0661 0.109 Uiso 1 1 calc R . . C26 C 0.2154(6) 0.6913(4) -0.0308(4) 0.089(3) Uani 1 1 d . . . H26A H 0.1698 0.7033 -0.0231 0.134 Uiso 1 1 calc R . . H26B H 0.2098 0.6722 -0.0657 0.134 Uiso 1 1 calc R . . H26C H 0.2459 0.7217 -0.0331 0.134 Uiso 1 1 calc R . . C27 C 0.5628(6) 0.5727(4) -0.0212(5) 0.101(4) Uani 1 1 d . . . H27A H 0.6080 0.5553 -0.0111 0.151 Uiso 1 1 calc R . . H27B H 0.5701 0.6103 -0.0263 0.151 Uiso 1 1 calc R . . H27C H 0.5391 0.5575 -0.0554 0.151 Uiso 1 1 calc R . . C28 C 0.6145(5) 0.5168(4) 0.0816(6) 0.102(4) Uani 1 1 d . . . H28A H 0.6388 0.5252 0.0505 0.153 Uiso 1 1 calc R . . H28B H 0.6125 0.4786 0.0860 0.153 Uiso 1 1 calc R . . H28C H 0.6396 0.5325 0.1151 0.153 Uiso 1 1 calc R . . C29 C 0.3884(4) 0.6600(3) 0.1888(3) 0.050(2) Uani 1 1 d . . . H29A H 0.3458 0.6657 0.1652 0.060 Uiso 1 1 calc R . . C30 C 0.4255(4) 0.7031(3) 0.2096(4) 0.057(2) Uani 1 1 d . . . C31 C 0.4870(5) 0.6962(3) 0.2430(4) 0.062(2) Uani 1 1 d . . . C32 C 0.5094(4) 0.6436(3) 0.2569(3) 0.051(2) Uani 1 1 d . . . C33 C 0.5731(5) 0.6306(3) 0.2917(4) 0.066(3) Uani 1 1 d . . . H33A H 0.6029 0.6582 0.3067 0.079 Uiso 1 1 calc R . . C34 C 0.5920(4) 0.5808(3) 0.3036(4) 0.061(2) Uani 1 1 d . . . H34A H 0.6345 0.5740 0.3269 0.073 Uiso 1 1 calc R . . C35 C 0.5493(4) 0.5377(3) 0.2820(3) 0.051(2) Uani 1 1 d . . . C36 C 0.5660(4) 0.4841(3) 0.2919(4) 0.057(2) Uani 1 1 d . . . C37 C 0.5187(4) 0.4464(3) 0.2703(3) 0.051(2) Uani 1 1 d . . . C38 C 0.4597(4) 0.4621(3) 0.2362(3) 0.0423(18) Uani 1 1 d . . . H38A H 0.4284 0.4356 0.2207 0.051 Uiso 1 1 calc R . . C39 C 0.4681(4) 0.6030(3) 0.2338(3) 0.0434(18) Uani 1 1 d . . . C40 C 0.4870(4) 0.5492(3) 0.2470(3) 0.0403(17) Uani 1 1 d . . . C41 C 0.3965(5) 0.7571(3) 0.1950(4) 0.080(3) Uani 1 1 d . . . H41A H 0.4281 0.7838 0.2132 0.119 Uiso 1 1 calc R . . H41B H 0.3507 0.7606 0.2071 0.119 Uiso 1 1 calc R . . H41C H 0.3917 0.7620 0.1551 0.119 Uiso 1 1 calc R . . C42 C 0.5309(6) 0.7423(3) 0.2655(5) 0.093(4) Uani 1 1 d . . . H42A H 0.5081 0.7751 0.2519 0.140 Uiso 1 1 calc R . . H42B H 0.5770 0.7401 0.2536 0.140 Uiso 1 1 calc R . . H42C H 0.5362 0.7418 0.3057 0.140 Uiso 1 1 calc R . . C43 C 0.6342(5) 0.4695(4) 0.3272(5) 0.084(3) Uani 1 1 d . . . H43A H 0.6601 0.5016 0.3390 0.125 Uiso 1 1 calc R . . H43B H 0.6621 0.4476 0.3059 0.125 Uiso 1 1 calc R . . H43C H 0.6243 0.4500 0.3595 0.125 Uiso 1 1 calc R . . C44 C 0.5312(5) 0.3885(3) 0.2796(4) 0.067(3) Uani 1 1 d . . . H44A H 0.4917 0.3687 0.2603 0.101 Uiso 1 1 calc R . . H44B H 0.5359 0.3810 0.3189 0.101 Uiso 1 1 calc R . . H44C H 0.5740 0.3783 0.2655 0.101 Uiso 1 1 calc R . . C45 C 0.0004(4) 0.2788(3) 0.0377(3) 0.0428(18) Uani 1 1 d . . . H45A H 0.0188 0.2978 0.0099 0.051 Uiso 1 1 calc R . . C46 C -0.0328(4) 0.2316(3) 0.0224(3) 0.0449(18) Uani 1 1 d . . . C47 C -0.0609(4) 0.2035(3) 0.0616(3) 0.051(2) Uani 1 1 d . . . C48 C -0.0540(4) 0.2243(3) 0.1153(3) 0.049(2) Uani 1 1 d . . . C49 C -0.0812(5) 0.1994(3) 0.1595(3) 0.065(3) Uani 1 1 d . . . H49A H -0.1058 0.1672 0.1532 0.078 Uiso 1 1 calc R . . C50 C -0.0729(5) 0.2203(4) 0.2095(3) 0.067(3) Uani 1 1 d . . . H50A H -0.0920 0.2024 0.2377 0.081 Uiso 1 1 calc R . . C51 C -0.0363(4) 0.2688(3) 0.2230(3) 0.053(2) Uani 1 1 d . . . C52 C -0.0255(4) 0.2917(3) 0.2757(3) 0.053(2) Uani 1 1 d . . . C53 C 0.0144(4) 0.3361(3) 0.2834(3) 0.0451(18) Uani 1 1 d . . . C54 C 0.0399(4) 0.3583(3) 0.2381(3) 0.0447(19) Uani 1 1 d . . . H54A H 0.0678 0.3890 0.2439 0.054 Uiso 1 1 calc R . . C55 C -0.0090(4) 0.2940(3) 0.1806(3) 0.0439(18) Uani 1 1 d . . . C56 C -0.0189(4) 0.2723(3) 0.1264(3) 0.0397(17) Uani 1 1 d . . . C57 C 0.0328(5) 0.3624(3) 0.3384(3) 0.057(2) Uani 1 1 d . . . H57A H 0.0116 0.3430 0.3662 0.085 Uiso 1 1 calc R . . H57B H 0.0151 0.3986 0.3363 0.085 Uiso 1 1 calc R . . H57C H 0.0835 0.3629 0.3485 0.085 Uiso 1 1 calc R . . C58 C -0.0563(5) 0.2670(4) 0.3225(3) 0.074(3) Uani 1 1 d . . . H58A H -0.0433 0.2877 0.3559 0.110 Uiso 1 1 calc R . . H58B H -0.0384 0.2311 0.3284 0.110 Uiso 1 1 calc R . . H58C H -0.1072 0.2660 0.3135 0.110 Uiso 1 1 calc R . . C59 C -0.0969(6) 0.1525(4) 0.0467(4) 0.075(3) Uani 1 1 d . . . H59A H -0.0966 0.1454 0.0076 0.112 Uiso 1 1 calc R . . H59B H -0.1452 0.1545 0.0541 0.112 Uiso 1 1 calc R . . H59C H -0.0726 0.1242 0.0685 0.112 Uiso 1 1 calc R . . C60 C -0.0382(5) 0.2125(4) -0.0353(3) 0.059(2) Uani 1 1 d . . . H60A H -0.0632 0.1790 -0.0387 0.089 Uiso 1 1 calc R . . H60B H 0.0086 0.2077 -0.0450 0.089 Uiso 1 1 calc R . . H60C H -0.0636 0.2384 -0.0600 0.089 Uiso 1 1 calc R . . C61 C 0.1211(4) 0.3887(3) 0.0033(3) 0.0441(18) Uani 1 1 d . . . H61A H 0.1620 0.3722 0.0212 0.053 Uiso 1 1 calc R . . C62 C 0.1208(4) 0.4051(3) -0.0509(3) 0.0465(19) Uani 1 1 d . . . C63 C 0.0629(4) 0.4293(3) -0.0775(3) 0.0454(19) Uani 1 1 d . . . C64 C 0.0058(4) 0.4361(3) -0.0492(3) 0.0453(19) Uani 1 1 d . . . C65 C -0.0570(5) 0.4614(3) -0.0720(3) 0.053(2) Uani 1 1 d . . . H65A H -0.0613 0.4735 -0.1088 0.063 Uiso 1 1 calc R . . C66 C -0.1088(5) 0.4688(3) -0.0450(4) 0.054(2) Uani 1 1 d . . . H66A H -0.1491 0.4864 -0.0626 0.065 Uiso 1 1 calc R . . C67 C -0.1075(4) 0.4516(3) 0.0103(3) 0.049(2) Uani 1 1 d . . . C68 C -0.1625(4) 0.4580(3) 0.0402(4) 0.057(2) Uani 1 1 d . . . C69 C -0.1552(4) 0.4389(3) 0.0925(4) 0.063(3) Uani 1 1 d . . . C70 C -0.0921(4) 0.4135(3) 0.1147(4) 0.057(2) Uani 1 1 d . . . H70A H -0.0882 0.4004 0.1510 0.068 Uiso 1 1 calc R . . C71 C 0.0107(4) 0.4184(3) 0.0054(3) 0.0362(16) Uani 1 1 d . . . C72 C -0.0462(4) 0.4260(3) 0.0354(3) 0.0424(18) Uani 1 1 d . . . C73 C 0.1853(5) 0.3946(4) -0.0775(4) 0.064(2) Uani 1 1 d . . . H73A H 0.1785 0.4085 -0.1150 0.095 Uiso 1 1 calc R . . H73B H 0.1936 0.3567 -0.0785 0.095 Uiso 1 1 calc R . . H73C H 0.2256 0.4118 -0.0562 0.095 Uiso 1 1 calc R . . C74 C 0.0593(5) 0.4495(3) -0.1350(3) 0.062(2) Uani 1 1 d . . . H74A H 0.1032 0.4417 -0.1488 0.093 Uiso 1 1 calc R . . H74B H 0.0518 0.4875 -0.1353 0.093 Uiso 1 1 calc R . . H74C H 0.0207 0.4324 -0.1584 0.093 Uiso 1 1 calc R . . C75 C -0.2280(4) 0.4851(4) 0.0161(4) 0.076(3) Uani 1 1 d . . . H75A H -0.2605 0.4860 0.0431 0.114 Uiso 1 1 calc R . . H75B H -0.2493 0.4661 -0.0167 0.114 Uiso 1 1 calc R . . H75C H -0.2171 0.5211 0.0060 0.114 Uiso 1 1 calc R . . C76 C -0.2106(5) 0.4424(4) 0.1304(5) 0.087(3) Uani 1 1 d . . . H76A H -0.2518 0.4605 0.1114 0.130 Uiso 1 1 calc R . . H76B H -0.1921 0.4619 0.1635 0.130 Uiso 1 1 calc R . . H76C H -0.2237 0.4069 0.1405 0.130 Uiso 1 1 calc R . . C77 C 0.2076(4) 0.2751(3) 0.2661(3) 0.050(2) Uani 1 1 d . . . H77A H 0.2286 0.2874 0.2359 0.060 Uiso 1 1 calc R . . C78 C 0.1595(4) 0.2341(3) 0.2568(3) 0.055(2) Uani 1 1 d . . . C79 C 0.1288(4) 0.2158(3) 0.3005(3) 0.055(2) Uani 1 1 d . . . C80 C 0.1463(4) 0.2397(3) 0.3515(3) 0.049(2) Uani 1 1 d . . . C81 C 0.1181(4) 0.2265(3) 0.4009(4) 0.059(2) Uani 1 1 d . . . H81A H 0.0842 0.1994 0.3991 0.070 Uiso 1 1 calc R . . C82 C 0.1373(4) 0.2505(3) 0.4489(4) 0.055(2) Uani 1 1 d . . . H82A H 0.1190 0.2384 0.4804 0.066 Uiso 1 1 calc R . . C83 C 0.1840(4) 0.2935(3) 0.4541(3) 0.0475(19) Uani 1 1 d . . . C84 C 0.2029(4) 0.3213(4) 0.5027(3) 0.060(2) Uani 1 1 d . . . C85 C 0.2500(5) 0.3621(4) 0.5032(4) 0.062(2) Uani 1 1 d . . . C86 C 0.2747(4) 0.3740(3) 0.4554(4) 0.058(2) Uani 1 1 d . . . H86A H 0.3063 0.4026 0.4561 0.069 Uiso 1 1 calc R . . C87 C 0.1945(4) 0.2815(3) 0.3565(3) 0.0419(18) Uani 1 1 d . . . C88 C 0.2128(4) 0.3083(3) 0.4076(3) 0.0454(19) Uani 1 1 d . . . C89 C 0.1444(5) 0.2107(4) 0.1999(4) 0.072(3) Uani 1 1 d . . . H89A H 0.1094 0.1828 0.1997 0.108 Uiso 1 1 calc R . . H89B H 0.1873 0.1959 0.1895 0.108 Uiso 1 1 calc R . . H89C H 0.1266 0.2381 0.1737 0.108 Uiso 1 1 calc R . . C90 C 0.0803(5) 0.1696(4) 0.2921(4) 0.072(3) Uani 1 1 d . . . H90A H 0.0750 0.1586 0.2536 0.107 Uiso 1 1 calc R . . H90B H 0.0347 0.1795 0.3017 0.107 Uiso 1 1 calc R . . H90C H 0.0995 0.1405 0.3155 0.107 Uiso 1 1 calc R . . C91 C 0.1712(5) 0.3065(4) 0.5532(4) 0.074(3) Uani 1 1 d . . . H91A H 0.1896 0.3296 0.5836 0.111 Uiso 1 1 calc R . . H91B H 0.1831 0.2699 0.5631 0.111 Uiso 1 1 calc R . . H91C H 0.1204 0.3102 0.5456 0.111 Uiso 1 1 calc R . . C92 C 0.2741(6) 0.3948(5) 0.5550(4) 0.087(3) Uani 1 1 d . . . H92A H 0.2522 0.3812 0.5856 0.131 Uiso 1 1 calc R . . H92B H 0.2605 0.4316 0.5482 0.131 Uiso 1 1 calc R . . H92C H 0.3249 0.3925 0.5641 0.131 Uiso 1 1 calc R . . C93 C 0.3835(6) 0.2657(4) 0.3668(5) 0.080(3) Uani 1 1 d . . . H93A H 0.3441 0.2469 0.3493 0.096 Uiso 1 1 calc R . . C94 C 0.4404(7) 0.2373(5) 0.3909(6) 0.102(4) Uani 1 1 d . . . C95 C 0.4981(7) 0.2634(5) 0.4146(5) 0.100(4) Uani 1 1 d . . . C96 C 0.4974(5) 0.3209(5) 0.4165(5) 0.087(3) Uani 1 1 d . . . C97 C 0.5518(7) 0.3544(6) 0.4405(6) 0.113(5) Uani 1 1 d . . . H97A H 0.5933 0.3386 0.4585 0.135 Uiso 1 1 calc R . . C98 C 0.5482(6) 0.4064(6) 0.4393(5) 0.105(4) Uani 1 1 d . . . H98A H 0.5869 0.4265 0.4558 0.126 Uiso 1 1 calc R . . C99 C 0.4863(5) 0.4328(4) 0.4134(4) 0.069(3) Uani 1 1 d . . . C100 C 0.4789(5) 0.4871(5) 0.4103(4) 0.075(3) Uani 1 1 d . . . C101 C 0.4173(5) 0.5086(3) 0.3820(4) 0.062(2) Uani 1 1 d . . . C102 C 0.3650(4) 0.4732(3) 0.3619(3) 0.050(2) Uani 1 1 d . . . H10A H 0.3223 0.4873 0.3441 0.060 Uiso 1 1 calc R . . C103 C 0.4355(5) 0.3458(4) 0.3908(4) 0.065(3) Uani 1 1 d . . . C104 C 0.4314(4) 0.4015(3) 0.3898(3) 0.053(2) Uani 1 1 d . . . C105 C 0.4358(8) 0.1781(4) 0.3904(7) 0.141(6) Uani 1 1 d . . . H10B H 0.4797 0.1633 0.4087 0.211 Uiso 1 1 calc R . . H10C H 0.4272 0.1656 0.3524 0.211 Uiso 1 1 calc R . . H10D H 0.3974 0.1669 0.4097 0.211 Uiso 1 1 calc R . . C106 C 0.5640(7) 0.2365(6) 0.4424(6) 0.135(6) Uani 1 1 d . . . H10E H 0.5590 0.1983 0.4381 0.202 Uiso 1 1 calc R . . H10F H 0.5714 0.2453 0.4815 0.202 Uiso 1 1 calc R . . H10G H 0.6040 0.2484 0.4255 0.202 Uiso 1 1 calc R . . C107 C 0.5368(6) 0.5248(5) 0.4354(5) 0.106(4) Uani 1 1 d . . . H10H H 0.5215 0.5612 0.4283 0.159 Uiso 1 1 calc R . . H10I H 0.5791 0.5184 0.4189 0.159 Uiso 1 1 calc R . . H10J H 0.5467 0.5190 0.4751 0.159 Uiso 1 1 calc R . . C108 C 0.4025(6) 0.5666(4) 0.3740(5) 0.082(3) Uani 1 1 d . . . H10K H 0.4432 0.5869 0.3903 0.123 Uiso 1 1 calc R . . H10L H 0.3622 0.5762 0.3918 0.123 Uiso 1 1 calc R . . H10M H 0.3925 0.5743 0.3347 0.123 Uiso 1 1 calc R . . C109 C 0.2567(7) 0.6714(6) 0.2684(6) 0.115(4) Uani 1 1 d D . . H10N H 0.2714 0.6978 0.2966 0.173 Uiso 1 1 calc R . . H10O H 0.2964 0.6490 0.2634 0.173 Uiso 1 1 calc R . . H10P H 0.2194 0.6498 0.2798 0.173 Uiso 1 1 calc R . . C110 C 0.2325(9) 0.6960(6) 0.2198(8) 0.109(6) Uani 1 1 d D . . C111 C 0.1114(12) 0.4763(7) 0.4280(7) 0.193(10) Uani 1 1 d . . . H11A H 0.1348 0.5033 0.4524 0.290 Uiso 1 1 calc R . . H11B H 0.0751 0.4927 0.4017 0.290 Uiso 1 1 calc R . . H11C H 0.1455 0.4591 0.4082 0.290 Uiso 1 1 calc R . . C112 C 0.0801(8) 0.4378(6) 0.4602(5) 0.114(4) Uani 1 1 d D . . C113 C 0.2558(17) 0.7947(12) 0.0551(16) 0.37(2) Uani 1 1 d DU . . H11D H 0.2764 0.8182 0.0303 0.562 Uiso 1 1 calc R . . H11E H 0.2106 0.7820 0.0370 0.562 Uiso 1 1 calc R . . H11F H 0.2869 0.7648 0.0648 0.562 Uiso 1 1 calc R . . C114 C -0.063(2) 0.5904(12) 0.3707(13) 0.35(3) Uani 1 1 d DU . . H11G H -0.0710 0.6178 0.3969 0.529 Uiso 1 1 calc R . . H11H H -0.0402 0.6058 0.3413 0.529 Uiso 1 1 calc R . . H11I H -0.0324 0.5633 0.3896 0.529 Uiso 1 1 calc R . . C115 C 0.2859(12) 0.6402(16) 0.4615(10) 0.34(2) Uani 1 1 d DU . . H11J H 0.3321 0.6241 0.4638 0.504 Uiso 1 1 calc R . . H11K H 0.2501 0.6136 0.4502 0.504 Uiso 1 1 calc R . . H11L H 0.2794 0.6543 0.4974 0.504 Uiso 1 1 calc R . . C116 C 0.149(2) 0.5204(15) 0.5751(13) 0.35(2) Uani 1 1 d DU . . H11M H 0.1920 0.5414 0.5782 0.525 Uiso 1 1 calc R . . H11N H 0.1446 0.4996 0.5413 0.525 Uiso 1 1 calc R . . H11O H 0.1513 0.4969 0.6067 0.525 Uiso 1 1 calc R . . C117 C 0.7131(11) 0.4726(9) 0.5189(8) 0.190(8) Uani 1 1 d DU . . H11P H 0.7571 0.4870 0.5375 0.285 Uiso 1 1 calc R . . H11Q H 0.6986 0.4430 0.5402 0.285 Uiso 1 1 calc R . . H11R H 0.6772 0.4999 0.5157 0.285 Uiso 1 1 calc R . . C118 C 0.7200(9) 0.3327(17) 0.1904(19) 0.49(3) Uani 1 1 d DU . . C119 C 0.5524(18) 0.6674(13) 0.4611(11) 0.246(13) Uani 1 1 d DU . . O1 O 0.2460(10) 0.8234(12) 0.1050(10) 0.322(13) Uani 1 1 d DU . . H1 H 0.2033 0.8290 0.1052 0.482 Uiso 1 1 calc R . . O2 O -0.132(2) 0.5657(14) 0.346(2) 0.55(3) Uani 1 1 d DU . . H2 H -0.1625 0.5720 0.3667 0.818 Uiso 1 1 calc R . . O3 O 0.2795(18) 0.6850(11) 0.4189(13) 0.45(2) Uani 1 1 d DU . . H3 H 0.2432 0.6807 0.3962 0.672 Uiso 1 1 calc R . . O4 O 0.086(3) 0.5572(19) 0.574(2) 0.61(3) Uani 1 1 d DU . . H4 H 0.0492 0.5396 0.5672 0.912 Uiso 1 1 calc R . . O5 O 0.7223(11) 0.4551(9) 0.4663(8) 0.291(10) Uani 1 1 d DU . . H5 H 0.7588 0.4684 0.4575 0.437 Uiso 1 1 calc R . . O6A O 0.7930(11) 0.3101(17) 0.195(2) 0.41(3) Uani 0.36(2) 1 d PDU . . O7A O 0.501(2) 0.6990(16) 0.4202(16) 0.225(16) Uani 0.36(2) 1 d PDU . . O7B O 0.5888(15) 0.7212(12) 0.4680(10) 0.237(13) Uani 0.64(2) 1 d PDU . . O8 O -0.1538(14) 0.447(2) 0.2756(10) 0.55(3) Uani 1 1 d . . . O9 O 0.2615(17) 0.4138(17) -0.2045(13) 0.52(3) Uani 1 1 d . . . O10 O 0.606(3) 0.235(2) 0.1259(15) 0.63(4) Uani 1 1 d . . . O6B O 0.6382(8) 0.339(2) 0.1719(12) 0.44(3) Uani 0.64(2) 1 d PDU . . N25 N 0.2266(12) 0.7223(10) 0.1870(9) 0.238(12) Uani 1 1 d D . . N26 N 0.0567(8) 0.4077(5) 0.4857(6) 0.145(5) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0393(4) 0.0422(4) 0.0474(4) 0.0020(3) 0.0095(3) -0.0015(3) Mo2 0.0466(4) 0.0456(4) 0.0496(4) 0.0031(3) 0.0097(3) 0.0051(3) Co1 0.0318(5) 0.0331(5) 0.0453(6) -0.0006(4) 0.0107(4) -0.0019(4) Co2 0.0330(5) 0.0435(6) 0.0340(5) 0.0074(4) 0.0068(4) -0.0048(4) Co3 0.0402(6) 0.0368(6) 0.0443(6) 0.0069(4) 0.0075(4) -0.0009(4) N1 0.033(3) 0.064(5) 0.056(4) 0.007(3) 0.019(3) 0.002(3) N2 0.058(5) 0.053(4) 0.040(4) 0.009(3) 0.003(3) -0.009(3) N3 0.044(4) 0.036(4) 0.085(6) 0.011(4) 0.001(4) -0.001(3) N4 0.081(6) 0.120(8) 0.068(6) -0.019(5) 0.012(5) -0.007(5) N5 0.053(5) 0.104(7) 0.082(6) 0.015(5) 0.021(4) 0.012(5) N6 0.068(5) 0.042(5) 0.126(7) 0.007(5) -0.023(5) 0.006(4) N7 0.064(5) 0.037(4) 0.058(4) 0.007(3) 0.001(4) 0.002(3) N8 0.041(4) 0.054(4) 0.048(4) 0.019(4) 0.008(3) 0.004(3) N9 0.051(4) 0.069(5) 0.046(4) 0.002(4) 0.010(3) -0.021(4) N10 0.075(5) 0.049(5) 0.071(5) -0.001(4) 0.005(4) 0.017(4) N11 0.116(8) 0.091(7) 0.083(7) -0.032(6) 0.025(6) 0.012(6) N12 0.074(7) 0.136(9) 0.147(10) 0.021(7) 0.053(7) 0.015(6) N13 0.038(4) 0.039(3) 0.047(4) 0.003(3) 0.007(3) -0.004(3) N14 0.038(4) 0.043(4) 0.058(4) -0.006(3) 0.017(3) -0.009(3) N15 0.042(4) 0.036(4) 0.047(4) -0.003(3) 0.010(3) 0.000(3) N16 0.033(3) 0.038(4) 0.051(4) -0.005(3) 0.007(3) -0.004(3) N17 0.037(3) 0.049(4) 0.036(4) 0.007(3) 0.009(3) 0.005(3) N18 0.042(3) 0.045(4) 0.035(4) -0.001(3) 0.010(3) -0.010(3) N19 0.040(4) 0.044(4) 0.037(3) 0.008(3) 0.007(3) -0.004(3) N20 0.041(4) 0.047(4) 0.048(4) -0.002(3) 0.014(3) -0.009(3) N21 0.049(4) 0.041(4) 0.050(4) 0.010(3) 0.013(3) -0.005(3) N22 0.049(4) 0.044(4) 0.054(4) 0.005(3) 0.005(3) -0.003(3) N23 0.067(5) 0.045(4) 0.068(5) 0.012(4) 0.022(4) 0.008(4) N24 0.043(4) 0.038(4) 0.049(4) 0.004(3) 0.005(3) 0.001(3) C1 0.031(4) 0.022(4) 0.044(4) 0.003(3) 0.012(3) -0.003(3) C2 0.024(4) 0.037(4) 0.036(4) 0.005(3) 0.005(3) -0.003(3) C3 0.029(4) 0.033(4) 0.028(4) 0.000(3) 0.005(3) -0.003(3) C4 0.049(5) 0.078(6) 0.060(6) -0.002(5) 0.013(4) -0.004(4) C5 0.050(5) 0.057(5) 0.056(5) 0.011(4) 0.017(4) 0.005(4) C6 0.041(5) 0.050(6) 0.071(6) -0.004(4) -0.004(4) 0.008(4) C7 0.037(4) 0.027(4) 0.042(4) 0.000(3) 0.013(3) -0.001(3) C8 0.030(4) 0.030(4) 0.035(4) 0.007(3) 0.003(3) -0.004(3) C9 0.032(4) 0.033(4) 0.028(4) 0.007(3) 0.000(3) 0.007(3) C10 0.054(5) 0.045(5) 0.056(5) -0.008(4) 0.008(4) 0.012(4) C11 0.078(6) 0.057(6) 0.061(6) -0.011(5) 0.015(5) 0.019(5) C12 0.068(7) 0.077(7) 0.096(8) 0.020(6) 0.042(6) 0.026(5) C13 0.042(5) 0.036(4) 0.050(5) 0.006(3) 0.002(4) -0.005(3) C14 0.050(5) 0.045(5) 0.057(5) 0.001(4) -0.004(4) -0.011(4) C15 0.076(6) 0.041(5) 0.061(6) 0.007(4) -0.020(5) -0.011(4) C16 0.075(6) 0.040(5) 0.054(5) 0.001(4) 0.006(5) -0.028(4) C17 0.109(9) 0.051(6) 0.058(6) -0.001(4) 0.014(6) -0.030(6) C18 0.118(9) 0.057(6) 0.054(6) -0.010(5) 0.036(6) -0.042(6) C19 0.075(6) 0.052(5) 0.061(6) -0.021(5) 0.032(5) -0.030(5) C20 0.077(7) 0.055(6) 0.082(7) -0.034(5) 0.050(6) -0.037(5) C21 0.052(5) 0.058(6) 0.100(8) -0.036(6) 0.034(6) -0.017(4) C22 0.036(5) 0.058(5) 0.068(6) -0.020(4) 0.021(4) -0.007(4) C23 0.054(5) 0.037(4) 0.044(5) 0.000(4) 0.007(4) -0.018(4) C24 0.052(5) 0.042(4) 0.048(5) -0.011(4) 0.018(4) -0.020(4) C25 0.070(6) 0.049(5) 0.089(7) 0.003(5) -0.019(5) 0.006(5) C26 0.117(9) 0.060(6) 0.080(7) 0.022(5) -0.023(6) -0.013(6) C27 0.114(9) 0.075(7) 0.134(10) -0.037(7) 0.091(8) -0.047(7) C28 0.047(6) 0.097(8) 0.172(12) -0.066(8) 0.047(7) -0.009(5) C29 0.047(5) 0.042(5) 0.059(5) -0.012(4) 0.002(4) 0.006(4) C30 0.060(5) 0.038(5) 0.069(6) -0.008(4) -0.003(5) 0.008(4) C31 0.072(6) 0.037(5) 0.074(6) -0.013(4) -0.001(5) -0.008(4) C32 0.055(5) 0.035(4) 0.059(5) -0.004(4) -0.002(4) 0.001(4) C33 0.069(6) 0.045(5) 0.075(6) -0.004(4) -0.017(5) -0.015(4) C34 0.055(5) 0.047(5) 0.073(6) -0.006(4) -0.019(4) -0.002(4) C35 0.045(5) 0.045(5) 0.061(5) -0.002(4) 0.005(4) -0.008(4) C36 0.051(5) 0.048(5) 0.070(6) 0.009(4) -0.002(4) 0.005(4) C37 0.053(5) 0.037(4) 0.060(5) 0.003(4) 0.001(4) 0.000(4) C38 0.040(4) 0.036(4) 0.052(5) -0.004(4) 0.010(4) -0.009(3) C39 0.043(4) 0.034(4) 0.054(5) -0.010(4) 0.008(4) -0.001(3) C40 0.037(4) 0.038(4) 0.047(4) 0.001(3) 0.010(3) 0.001(3) C41 0.091(7) 0.044(5) 0.096(8) -0.010(5) -0.011(6) 0.017(5) C42 0.104(8) 0.037(5) 0.124(9) -0.010(5) -0.037(7) -0.008(5) C43 0.074(7) 0.051(6) 0.116(9) 0.009(6) -0.022(6) 0.005(5) C44 0.066(6) 0.037(5) 0.096(7) 0.010(5) 0.000(5) 0.001(4) C45 0.046(4) 0.055(5) 0.031(4) 0.001(4) 0.015(3) 0.007(4) C46 0.044(4) 0.055(5) 0.036(4) -0.002(4) 0.008(3) 0.006(4) C47 0.052(5) 0.060(5) 0.043(5) -0.005(4) 0.009(4) -0.008(4) C48 0.055(5) 0.050(5) 0.044(5) 0.003(4) 0.008(4) -0.012(4) C49 0.092(7) 0.062(6) 0.045(5) -0.007(4) 0.019(5) -0.045(5) C50 0.090(7) 0.074(6) 0.040(5) 0.004(4) 0.019(5) -0.042(5) C51 0.065(5) 0.061(5) 0.034(4) 0.004(4) 0.011(4) -0.024(4) C52 0.062(5) 0.060(5) 0.038(5) 0.007(4) 0.015(4) -0.020(4) C53 0.051(5) 0.048(5) 0.036(4) 0.008(3) 0.006(3) -0.009(4) C54 0.041(4) 0.044(4) 0.049(5) 0.000(4) 0.007(4) -0.014(3) C55 0.042(4) 0.049(5) 0.042(4) 0.008(4) 0.010(3) -0.005(4) C56 0.042(4) 0.050(5) 0.028(4) 0.003(3) 0.008(3) -0.002(3) C57 0.066(6) 0.059(5) 0.045(5) 0.002(4) 0.007(4) -0.010(4) C58 0.103(8) 0.083(7) 0.037(5) 0.000(4) 0.021(5) -0.040(6) C59 0.101(8) 0.077(7) 0.049(5) -0.009(5) 0.019(5) -0.029(6) C60 0.065(6) 0.073(6) 0.041(5) 0.000(4) 0.014(4) -0.002(5) C61 0.045(4) 0.042(4) 0.047(5) 0.003(3) 0.010(4) -0.006(3) C62 0.054(5) 0.045(5) 0.043(5) 0.007(4) 0.014(4) -0.011(4) C63 0.059(5) 0.037(4) 0.041(4) 0.004(3) 0.009(4) -0.009(4) C64 0.053(5) 0.029(4) 0.050(5) 0.002(3) -0.006(4) -0.008(3) C65 0.063(6) 0.040(5) 0.053(5) 0.003(4) 0.002(4) -0.003(4) C66 0.057(5) 0.038(4) 0.061(6) 0.001(4) -0.013(4) 0.005(4) C67 0.040(4) 0.039(4) 0.065(5) -0.012(4) -0.003(4) -0.004(3) C68 0.050(5) 0.052(5) 0.070(6) -0.007(5) 0.009(4) -0.011(4) C69 0.040(5) 0.056(5) 0.100(8) -0.023(5) 0.029(5) -0.006(4) C70 0.055(5) 0.056(5) 0.064(5) 0.000(4) 0.019(4) -0.014(4) C71 0.041(4) 0.031(4) 0.036(4) 0.000(3) 0.003(3) -0.004(3) C72 0.041(4) 0.035(4) 0.049(5) -0.003(3) 0.000(4) -0.009(3) C73 0.071(6) 0.069(6) 0.055(5) 0.006(4) 0.025(5) -0.009(5) C74 0.078(6) 0.061(6) 0.045(5) 0.006(4) 0.003(4) -0.007(5) C75 0.048(5) 0.073(6) 0.104(8) -0.018(6) -0.004(5) 0.009(5) C76 0.066(6) 0.089(8) 0.114(9) -0.015(6) 0.045(6) -0.010(6) C77 0.060(5) 0.045(5) 0.050(5) 0.003(4) 0.018(4) -0.013(4) C78 0.063(5) 0.052(5) 0.050(5) 0.005(4) 0.009(4) -0.009(4) C79 0.065(5) 0.045(5) 0.057(5) 0.007(4) 0.013(4) -0.012(4) C80 0.050(5) 0.044(5) 0.055(5) 0.010(4) 0.015(4) -0.008(4) C81 0.057(5) 0.054(5) 0.065(6) 0.020(5) 0.009(4) -0.006(4) C82 0.041(5) 0.071(6) 0.053(5) 0.020(5) 0.011(4) -0.003(4) C83 0.038(4) 0.053(5) 0.050(5) 0.011(4) 0.000(4) 0.003(4) C84 0.046(5) 0.080(6) 0.054(5) 0.010(5) 0.005(4) 0.009(5) C85 0.054(5) 0.076(6) 0.054(5) -0.010(5) 0.006(4) -0.007(5) C86 0.055(5) 0.053(5) 0.065(6) 0.001(5) 0.010(4) -0.006(4) C87 0.037(4) 0.038(4) 0.050(5) 0.011(4) 0.003(3) -0.002(3) C88 0.041(4) 0.046(5) 0.049(5) 0.012(4) 0.008(4) 0.000(4) C89 0.089(7) 0.072(6) 0.056(6) -0.006(5) 0.013(5) -0.029(5) C90 0.080(7) 0.067(6) 0.070(6) 0.000(5) 0.018(5) -0.033(5) C91 0.062(6) 0.110(8) 0.050(5) 0.014(5) 0.010(4) -0.004(5) C92 0.091(8) 0.103(8) 0.067(7) 0.000(6) 0.003(6) -0.022(6) C93 0.086(7) 0.058(6) 0.101(8) 0.020(6) 0.033(6) 0.010(5) C94 0.086(9) 0.077(8) 0.150(12) 0.046(8) 0.039(8) 0.026(7) C95 0.099(9) 0.093(9) 0.110(9) 0.060(7) 0.027(8) 0.055(8) C96 0.055(6) 0.113(9) 0.094(8) 0.044(7) 0.013(6) 0.020(6) C97 0.076(9) 0.136(12) 0.118(11) 0.059(9) -0.015(7) 0.023(9) C98 0.055(7) 0.145(13) 0.106(9) 0.023(9) -0.023(6) -0.015(7) C99 0.059(6) 0.077(7) 0.068(6) 0.002(5) -0.004(5) -0.006(5) C100 0.055(6) 0.102(9) 0.064(6) -0.021(6) 0.002(5) -0.027(6) C101 0.061(6) 0.057(6) 0.071(6) -0.017(5) 0.017(5) -0.019(5) C102 0.043(5) 0.053(5) 0.057(5) -0.009(4) 0.013(4) -0.003(4) C103 0.054(6) 0.072(7) 0.070(6) 0.027(5) 0.014(5) 0.020(5) C104 0.040(5) 0.066(6) 0.050(5) 0.010(4) 0.001(4) -0.002(4) C105 0.185(15) 0.062(8) 0.195(15) 0.061(9) 0.093(13) 0.055(9) C106 0.128(11) 0.122(11) 0.157(13) 0.069(10) 0.028(10) 0.060(9) C107 0.078(8) 0.133(11) 0.103(9) -0.025(8) 0.000(7) -0.043(7) C108 0.094(8) 0.055(6) 0.104(8) -0.017(5) 0.033(6) -0.015(5) C109 0.118(11) 0.103(10) 0.127(12) -0.013(9) 0.025(9) 0.002(8) C110 0.104(11) 0.070(8) 0.173(19) -0.011(9) 0.090(13) 0.018(7) C111 0.30(3) 0.165(17) 0.123(13) -0.003(12) 0.071(16) -0.100(18) C112 0.129(12) 0.128(12) 0.083(9) -0.001(8) 0.014(8) -0.030(10) C113 0.26(3) 0.19(2) 0.59(5) -0.14(3) -0.22(3) 0.03(2) C114 0.68(7) 0.19(3) 0.19(2) 0.05(2) 0.06(4) 0.25(4) C115 0.145(18) 0.70(6) 0.15(2) -0.13(3) -0.023(15) 0.14(3) C116 0.58(7) 0.32(5) 0.19(2) -0.01(3) 0.18(4) -0.13(4) C117 0.172(18) 0.22(2) 0.172(17) 0.006(16) 0.006(16) 0.013(16) C118 0.107(11) 0.61(5) 0.73(5) 0.57(4) -0.02(2) -0.011(19) C119 0.27(3) 0.35(4) 0.139(18) -0.04(2) 0.078(19) 0.00(2) O1 0.155(14) 0.43(4) 0.35(3) 0.11(2) -0.035(18) 0.05(2) O2 0.77(8) 0.26(3) 0.62(6) 0.08(4) 0.17(5) 0.02(4) O3 0.51(4) 0.38(4) 0.41(4) -0.18(3) -0.07(3) 0.20(3) O4 0.85(9) 0.48(6) 0.52(5) -0.01(4) 0.20(5) 0.12(5) O5 0.28(2) 0.34(2) 0.28(2) -0.080(19) 0.102(18) -0.104(18) O6A 0.059(11) 0.43(5) 0.70(7) 0.50(5) -0.12(2) -0.075(18) O7A 0.37(4) 0.17(3) 0.16(3) 0.03(2) 0.10(2) -0.06(3) O7B 0.24(2) 0.33(3) 0.172(19) 0.07(2) 0.132(16) -0.01(2) O8 0.30(3) 1.11(10) 0.22(2) -0.13(4) -0.04(2) -0.21(4) O9 0.43(4) 0.76(7) 0.39(4) -0.04(4) 0.12(3) -0.34(5) O10 0.81(9) 0.71(8) 0.39(4) 0.29(5) 0.15(5) 0.50(7) O6B 0.086(10) 0.99(7) 0.24(3) 0.37(4) 0.070(14) 0.11(2) N25 0.141(15) 0.33(4) 0.25(3) -0.08(2) 0.045(17) 0.01(2) N26 0.172(13) 0.135(11) 0.139(11) 0.016(9) 0.058(10) -0.038(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C4 2.135(10) . ? Mo1 C2 2.137(7) . ? Mo1 C3 2.139(7) . ? Mo1 C1 2.152(7) . ? Mo1 C6 2.156(9) . ? Mo1 C5 2.171(9) . ? Mo2 C9 2.123(7) . ? Mo2 C11 2.133(10) . ? Mo2 C12 2.135(10) . ? Mo2 C7 2.142(8) . ? Mo2 C10 2.147(9) . ? Mo2 C8 2.157(8) . ? Co1 N7 1.997(8) . ? Co1 N1 2.038(8) . ? Co1 N14 2.079(6) . ? Co1 N15 2.094(6) . ? Co1 N13 2.143(6) . ? Co1 N16 2.158(6) . ? Co2 N2 2.008(7) . ? Co2 N8 2.036(8) . ? Co2 N20 2.089(6) . ? Co2 N17 2.102(6) . ? Co2 N18 2.145(6) . ? Co2 N19 2.154(6) . ? Co3 N9 1.994(8) . ? Co3 N3 1.996(9) . ? Co3 N23 2.045(7) . ? Co3 N22 2.072(7) . ? Co3 N24 2.143(6) . ? Co3 N21 2.155(6) . ? N1 C1 1.130(9) . ? N2 C2 1.136(9) . ? N3 C3 1.133(9) . ? N4 C4 1.150(11) . ? N5 C5 1.126(10) . ? N6 C6 1.141(11) . ? N7 C7 1.119(9) . ? N8 C8 1.128(9) . ? N9 C9 1.134(9) . ? N10 C10 1.137(10) . ? N11 C11 1.138(11) . ? N12 C12 1.166(12) . ? N13 C13 1.314(9) . ? N13 C23 1.340(9) . ? N14 C22 1.325(10) . ? N14 C24 1.357(10) . ? N15 C29 1.334(9) . ? N15 C39 1.349(9) . ? N16 C38 1.328(9) . ? N16 C40 1.345(9) . ? N17 C45 1.321(9) . ? N17 C56 1.355(9) . ? N18 C54 1.326(9) . ? N18 C55 1.341(9) . ? N19 C61 1.334(9) . ? N19 C71 1.342(9) . ? N20 C70 1.319(10) . ? N20 C72 1.359(9) . ? N21 C77 1.309(10) . ? N21 C87 1.350(9) . ? N22 C86 1.320(10) . ? N22 C88 1.357(10) . ? N23 C103 1.335(12) . ? N23 C93 1.343(11) . ? N24 C102 1.322(10) . ? N24 C104 1.348(10) . ? C13 C14 1.404(11) . ? C14 C15 1.389(12) . ? C14 C25 1.499(12) . ? C15 C16 1.422(13) . ? C15 C26 1.490(12) . ? C16 C23 1.393(11) . ? C16 C17 1.436(13) . ? C17 C18 1.341(14) . ? C18 C19 1.436(14) . ? C19 C24 1.385(11) . ? C19 C20 1.429(14) . ? C20 C21 1.356(14) . ? C20 C27 1.527(12) . ? C21 C22 1.370(12) . ? C21 C28 1.502(13) . ? C23 C24 1.458(11) . ? C29 C30 1.372(11) . ? C30 C31 1.360(12) . ? C30 C41 1.510(11) . ? C31 C32 1.433(11) . ? C31 C42 1.510(12) . ? C32 C39 1.380(10) . ? C32 C33 1.439(12) . ? C33 C34 1.340(12) . ? C34 C35 1.430(11) . ? C35 C40 1.412(11) . ? C35 C36 1.415(11) . ? C36 C37 1.381(11) . ? C36 C43 1.522(12) . ? C37 C38 1.378(10) . ? C37 C44 1.505(11) . ? C39 C40 1.444(10) . ? C45 C46 1.388(11) . ? C46 C47 1.374(11) . ? C46 C60 1.492(10) . ? C47 C48 1.413(11) . ? C47 C59 1.495(12) . ? C48 C56 1.406(10) . ? C48 C49 1.426(11) . ? C49 C50 1.331(11) . ? C50 C51 1.439(11) . ? C51 C55 1.393(10) . ? C51 C52 1.412(11) . ? C52 C53 1.368(11) . ? C52 C58 1.508(10) . ? C53 C54 1.401(10) . ? C53 C57 1.509(11) . ? C55 C56 1.434(10) . ? C61 C62 1.398(10) . ? C62 C63 1.361(11) . ? C62 C73 1.517(11) . ? C63 C64 1.400(11) . ? C63 C74 1.498(11) . ? C64 C71 1.408(10) . ? C64 C65 1.422(11) . ? C65 C66 1.295(12) . ? C66 C67 1.428(12) . ? C67 C68 1.389(12) . ? C67 C72 1.417(11) . ? C68 C69 1.365(13) . ? C68 C75 1.493(12) . ? C69 C70 1.422(12) . ? C69 C76 1.522(12) . ? C71 C72 1.427(10) . ? C77 C78 1.398(11) . ? C78 C79 1.385(11) . ? C78 C89 1.512(12) . ? C79 C80 1.393(11) . ? C79 C90 1.503(11) . ? C80 C87 1.410(10) . ? C80 C81 1.442(11) . ? C81 C82 1.337(12) . ? C82 C83 1.415(11) . ? C83 C84 1.395(12) . ? C83 C88 1.397(10) . ? C84 C85 1.383(12) . ? C84 C91 1.510(12) . ? C85 C86 1.365(12) . ? C85 C92 1.540(13) . ? C87 C88 1.431(11) . ? C93 C94 1.380(15) . ? C94 C95 1.359(18) . ? C94 C105 1.512(16) . ? C95 C96 1.466(17) . ? C95 C106 1.524(16) . ? C96 C97 1.419(18) . ? C96 C103 1.423(13) . ? C97 C98 1.325(18) . ? C98 C99 1.442(15) . ? C99 C104 1.389(12) . ? C99 C100 1.391(14) . ? C100 C101 1.405(14) . ? C100 C107 1.539(13) . ? C101 C102 1.395(11) . ? C101 C108 1.512(13) . ? C103 C104 1.422(13) . ? C109 C110 1.373(15) . ? C110 N25 1.043(17) . ? C111 C112 1.45(2) . ? C112 N26 1.126(13) . ? C113 O1 1.466(19) . ? C114 O2 1.53(2) . ? C115 O3 1.544(19) . ? C116 O4 1.54(2) . ? C117 O5 1.405(16) . ? C118 O6A 1.52(2) . ? C118 O6B 1.593(17) . ? C119 O7B 1.538(19) . ? C119 O7A 1.54(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Mo1 C2 91.1(3) . . ? C4 Mo1 C3 178.1(3) . . ? C2 Mo1 C3 87.2(2) . . ? C4 Mo1 C1 95.0(3) . . ? C2 Mo1 C1 92.0(2) . . ? C3 Mo1 C1 85.7(2) . . ? C4 Mo1 C6 89.8(3) . . ? C2 Mo1 C6 86.0(3) . . ? C3 Mo1 C6 89.4(3) . . ? C1 Mo1 C6 174.8(3) . . ? C4 Mo1 C5 90.7(3) . . ? C2 Mo1 C5 178.2(3) . . ? C3 Mo1 C5 91.1(3) . . ? C1 Mo1 C5 88.5(3) . . ? C6 Mo1 C5 93.3(3) . . ? C9 Mo2 C11 88.9(3) . . ? C9 Mo2 C12 94.6(3) . . ? C11 Mo2 C12 95.0(4) . . ? C9 Mo2 C7 87.2(3) . . ? C11 Mo2 C7 89.8(3) . . ? C12 Mo2 C7 174.9(4) . . ? C9 Mo2 C10 173.2(3) . . ? C11 Mo2 C10 90.9(3) . . ? C12 Mo2 C10 92.2(3) . . ? C7 Mo2 C10 86.0(3) . . ? C9 Mo2 C8 85.7(2) . . ? C11 Mo2 C8 174.5(3) . . ? C12 Mo2 C8 86.3(4) . . ? C7 Mo2 C8 89.0(2) . . ? C10 Mo2 C8 94.4(3) . . ? N7 Co1 N1 89.3(2) . . ? N7 Co1 N14 172.7(3) . . ? N1 Co1 N14 90.0(2) . . ? N7 Co1 N15 94.7(2) . . ? N1 Co1 N15 170.8(2) . . ? N14 Co1 N15 87.1(2) . . ? N7 Co1 N13 94.8(2) . . ? N1 Co1 N13 98.4(2) . . ? N14 Co1 N13 78.1(2) . . ? N15 Co1 N13 89.5(2) . . ? N7 Co1 N16 95.5(2) . . ? N1 Co1 N16 94.3(2) . . ? N14 Co1 N16 91.8(2) . . ? N15 Co1 N16 77.1(2) . . ? N13 Co1 N16 163.7(2) . . ? N2 Co2 N8 88.2(3) . . ? N2 Co2 N20 167.9(2) . . ? N8 Co2 N20 91.0(2) . . ? N2 Co2 N17 96.1(2) . . ? N8 Co2 N17 167.1(2) . . ? N20 Co2 N17 87.4(2) . . ? N2 Co2 N18 96.5(2) . . ? N8 Co2 N18 90.4(2) . . ? N20 Co2 N18 95.6(2) . . ? N17 Co2 N18 77.1(2) . . ? N2 Co2 N19 90.5(2) . . ? N8 Co2 N19 99.1(2) . . ? N20 Co2 N19 77.7(2) . . ? N17 Co2 N19 93.0(2) . . ? N18 Co2 N19 168.4(2) . . ? N9 Co3 N3 92.1(3) . . ? N9 Co3 N23 169.7(3) . . ? N3 Co3 N23 91.2(3) . . ? N9 Co3 N22 91.9(3) . . ? N3 Co3 N22 168.4(3) . . ? N23 Co3 N22 86.7(3) . . ? N9 Co3 N24 92.1(2) . . ? N3 Co3 N24 94.1(2) . . ? N23 Co3 N24 77.9(3) . . ? N22 Co3 N24 96.6(2) . . ? N9 Co3 N21 92.6(2) . . ? N3 Co3 N21 90.7(2) . . ? N23 Co3 N21 97.1(3) . . ? N22 Co3 N21 78.3(2) . . ? N24 Co3 N21 173.2(2) . . ? C1 N1 Co1 164.6(6) . . ? C2 N2 Co2 159.5(6) . . ? C3 N3 Co3 167.7(6) . . ? C7 N7 Co1 169.4(7) . . ? C8 N8 Co2 166.6(6) . . ? C9 N9 Co3 170.2(6) . . ? C13 N13 C23 118.3(6) . . ? C13 N13 Co1 128.0(5) . . ? C23 N13 Co1 113.5(5) . . ? C22 N14 C24 116.9(7) . . ? C22 N14 Co1 127.8(6) . . ? C24 N14 Co1 115.3(5) . . ? C29 N15 C39 117.0(6) . . ? C29 N15 Co1 127.3(5) . . ? C39 N15 Co1 115.2(5) . . ? C38 N16 C40 117.5(6) . . ? C38 N16 Co1 129.1(5) . . ? C40 N16 Co1 112.9(5) . . ? C45 N17 C56 116.5(6) . . ? C45 N17 Co2 128.4(5) . . ? C56 N17 Co2 115.1(5) . . ? C54 N18 C55 117.5(6) . . ? C54 N18 Co2 128.3(5) . . ? C55 N18 Co2 114.2(5) . . ? C61 N19 C71 116.6(6) . . ? C61 N19 Co2 130.3(5) . . ? C71 N19 Co2 113.1(4) . . ? C70 N20 C72 116.7(7) . . ? C70 N20 Co2 128.6(6) . . ? C72 N20 Co2 114.7(5) . . ? C77 N21 C87 118.3(6) . . ? C77 N21 Co3 129.3(5) . . ? C87 N21 Co3 112.4(5) . . ? C86 N22 C88 117.2(7) . . ? C86 N22 Co3 127.9(6) . . ? C88 N22 Co3 114.9(5) . . ? C103 N23 C93 119.6(8) . . ? C103 N23 Co3 115.2(6) . . ? C93 N23 Co3 125.2(7) . . ? C102 N24 C104 117.4(7) . . ? C102 N24 Co3 129.5(5) . . ? C104 N24 Co3 113.1(5) . . ? N1 C1 Mo1 166.7(6) . . ? N2 C2 Mo1 178.7(6) . . ? N3 C3 Mo1 171.0(6) . . ? N4 C4 Mo1 176.3(9) . . ? N5 C5 Mo1 179.3(8) . . ? N6 C6 Mo1 174.8(7) . . ? N7 C7 Mo2 174.0(7) . . ? N8 C8 Mo2 170.3(6) . . ? N9 C9 Mo2 167.6(6) . . ? N10 C10 Mo2 177.4(8) . . ? N11 C11 Mo2 177.2(9) . . ? N12 C12 Mo2 178.2(11) . . ? N13 C13 C14 124.6(7) . . ? C15 C14 C13 117.7(8) . . ? C15 C14 C25 123.3(8) . . ? C13 C14 C25 119.0(8) . . ? C14 C15 C16 118.1(7) . . ? C14 C15 C26 120.4(9) . . ? C16 C15 C26 121.5(9) . . ? C23 C16 C15 118.8(8) . . ? C23 C16 C17 117.4(9) . . ? C15 C16 C17 123.7(9) . . ? C18 C17 C16 121.1(10) . . ? C17 C18 C19 123.3(9) . . ? C24 C19 C20 117.1(9) . . ? C24 C19 C18 116.8(9) . . ? C20 C19 C18 126.1(9) . . ? C21 C20 C19 118.9(8) . . ? C21 C20 C27 122.3(10) . . ? C19 C20 C27 118.8(11) . . ? C20 C21 C22 119.3(9) . . ? C20 C21 C28 121.3(10) . . ? C22 C21 C28 119.3(11) . . ? N14 C22 C21 124.4(9) . . ? N13 C23 C16 122.4(8) . . ? N13 C23 C24 116.8(7) . . ? C16 C23 C24 120.8(7) . . ? N14 C24 C19 123.3(8) . . ? N14 C24 C23 116.2(6) . . ? C19 C24 C23 120.4(8) . . ? N15 C29 C30 124.2(7) . . ? C31 C30 C29 119.3(7) . . ? C31 C30 C41 121.9(8) . . ? C29 C30 C41 118.8(8) . . ? C30 C31 C32 118.4(7) . . ? C30 C31 C42 121.4(8) . . ? C32 C31 C42 120.2(8) . . ? C39 C32 C31 117.6(7) . . ? C39 C32 C33 118.1(7) . . ? C31 C32 C33 124.3(7) . . ? C34 C33 C32 122.2(8) . . ? C33 C34 C35 121.3(8) . . ? C40 C35 C36 117.3(7) . . ? C40 C35 C34 117.9(7) . . ? C36 C35 C34 124.8(7) . . ? C37 C36 C35 118.8(7) . . ? C37 C36 C43 121.7(7) . . ? C35 C36 C43 119.5(8) . . ? C38 C37 C36 118.7(7) . . ? C38 C37 C44 118.6(7) . . ? C36 C37 C44 122.6(7) . . ? N16 C38 C37 124.5(7) . . ? N15 C39 C32 123.4(7) . . ? N15 C39 C40 116.2(6) . . ? C32 C39 C40 120.4(7) . . ? N16 C40 C35 123.0(6) . . ? N16 C40 C39 117.0(6) . . ? C35 C40 C39 120.0(7) . . ? N17 C45 C46 125.8(7) . . ? C47 C46 C45 118.4(7) . . ? C47 C46 C60 121.2(7) . . ? C45 C46 C60 120.4(7) . . ? C46 C47 C48 117.9(7) . . ? C46 C47 C59 119.9(7) . . ? C48 C47 C59 122.2(7) . . ? C56 C48 C47 119.1(7) . . ? C56 C48 C49 117.3(7) . . ? C47 C48 C49 123.6(7) . . ? C50 C49 C48 121.4(7) . . ? C49 C50 C51 123.2(7) . . ? C55 C51 C52 118.5(7) . . ? C55 C51 C50 116.8(7) . . ? C52 C51 C50 124.7(7) . . ? C53 C52 C51 118.3(7) . . ? C53 C52 C58 121.2(7) . . ? C51 C52 C58 120.5(7) . . ? C52 C53 C54 118.7(7) . . ? C52 C53 C57 123.2(7) . . ? C54 C53 C57 118.1(7) . . ? N18 C54 C53 123.8(7) . . ? N18 C55 C51 123.0(7) . . ? N18 C55 C56 116.6(6) . . ? C51 C55 C56 120.4(7) . . ? N17 C56 C48 122.3(6) . . ? N17 C56 C55 116.8(6) . . ? C48 C56 C55 120.9(6) . . ? N19 C61 C62 124.5(7) . . ? C63 C62 C61 119.0(7) . . ? C63 C62 C73 123.1(7) . . ? C61 C62 C73 117.9(7) . . ? C62 C63 C64 118.2(7) . . ? C62 C63 C74 122.2(7) . . ? C64 C63 C74 119.6(7) . . ? C63 C64 C71 119.1(7) . . ? C63 C64 C65 123.6(7) . . ? C71 C64 C65 117.3(7) . . ? C66 C65 C64 123.1(8) . . ? C65 C66 C67 122.5(8) . . ? C68 C67 C72 118.8(8) . . ? C68 C67 C66 124.0(8) . . ? C72 C67 C66 117.2(7) . . ? C69 C68 C67 118.4(8) . . ? C69 C68 C75 120.5(8) . . ? C67 C68 C75 121.1(9) . . ? C68 C69 C70 119.4(8) . . ? C68 C69 C76 124.8(9) . . ? C70 C69 C76 115.8(9) . . ? N20 C70 C69 123.8(8) . . ? N19 C71 C64 122.7(6) . . ? N19 C71 C72 117.3(6) . . ? C64 C71 C72 120.1(7) . . ? N20 C72 C67 123.0(7) . . ? N20 C72 C71 117.1(6) . . ? C67 C72 C71 119.9(7) . . ? N21 C77 C78 124.2(7) . . ? C79 C78 C77 118.3(8) . . ? C79 C78 C89 122.8(7) . . ? C77 C78 C89 118.9(7) . . ? C78 C79 C80 118.6(7) . . ? C78 C79 C90 119.0(8) . . ? C80 C79 C90 122.3(7) . . ? C79 C80 C87 118.8(7) . . ? C79 C80 C81 125.8(7) . . ? C87 C80 C81 115.5(7) . . ? C82 C81 C80 123.2(8) . . ? C81 C82 C83 121.8(8) . . ? C84 C83 C88 118.8(7) . . ? C84 C83 C82 123.7(8) . . ? C88 C83 C82 117.5(7) . . ? C85 C84 C83 118.6(8) . . ? C85 C84 C91 121.9(9) . . ? C83 C84 C91 119.5(8) . . ? C86 C85 C84 118.2(8) . . ? C86 C85 C92 119.5(8) . . ? C84 C85 C92 122.3(8) . . ? N22 C86 C85 125.3(8) . . ? N21 C87 C80 121.8(7) . . ? N21 C87 C88 117.2(6) . . ? C80 C87 C88 121.0(7) . . ? N22 C88 C83 121.8(7) . . ? N22 C88 C87 117.2(7) . . ? C83 C88 C87 121.0(7) . . ? N23 C93 C94 123.5(11) . . ? C95 C94 C93 119.2(11) . . ? C95 C94 C105 122.4(12) . . ? C93 C94 C105 118.4(14) . . ? C94 C95 C96 119.4(10) . . ? C94 C95 C106 124.0(12) . . ? C96 C95 C106 116.5(13) . . ? C97 C96 C103 116.7(11) . . ? C97 C96 C95 127.1(11) . . ? C103 C96 C95 116.2(11) . . ? C98 C97 C96 123.8(11) . . ? C97 C98 C99 120.9(11) . . ? C104 C99 C100 118.7(9) . . ? C104 C99 C98 117.2(10) . . ? C100 C99 C98 124.1(10) . . ? C99 C100 C101 119.3(8) . . ? C99 C100 C107 122.3(10) . . ? C101 C100 C107 118.4(10) . . ? C102 C101 C100 116.6(9) . . ? C102 C101 C108 118.0(9) . . ? C100 C101 C108 125.4(9) . . ? N24 C102 C101 125.1(8) . . ? N23 C103 C104 118.4(7) . . ? N23 C103 C96 122.1(10) . . ? C104 C103 C96 119.5(10) . . ? N24 C104 C99 122.8(8) . . ? N24 C104 C103 115.3(7) . . ? C99 C104 C103 121.8(8) . . ? N25 C110 C109 163(3) . . ? N26 C112 C111 179(2) . . ? O6A C118 O6B 160(5) . . ? O7B C119 O7A 82(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 22.41 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.233 _refine_diff_density_min -0.623 _refine_diff_density_rms 0.111 data_Ni3Mo2TBP _database_code_depnum_ccdc_archive 'CCDC 724501' #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C115 H139 Mo2 N25 Ni3 O15' _chemical_formula_weight 2479.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.394(2) _cell_length_b 25.236(3) _cell_length_c 24.423(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.144(2) _cell_angle_gamma 90.00 _cell_volume 11833(2) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 32592 _cell_measurement_theta_min 2.2631 _cell_measurement_theta_max 17.6378 _exptl_crystal_description column _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5168 _exptl_absorpt_coefficient_mu 0.747 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7543 _exptl_absorpt_correction_T_max 0.9157 _exptl_absorpt_process_details 'SADABS: Bruker,2000' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 'BRUKER APEX' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 112493 _diffrn_reflns_av_R_equivalents 0.1313 _diffrn_reflns_av_sigmaI/netI 0.1098 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 25.00 _reflns_number_total 20830 _reflns_number_gt 9756 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Diomand _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1331P)^2^+20.7722P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20830 _refine_ls_number_parameters 1442 _refine_ls_number_restraints 125 _refine_ls_R_factor_all 0.1779 _refine_ls_R_factor_gt 0.0772 _refine_ls_wR_factor_ref 0.2758 _refine_ls_wR_factor_gt 0.1924 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.005 _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 0.13824(5) 0.52401(4) 0.25659(4) 0.0621(3) Uani 1 1 d . . . Mo2 Mo 0.32279(4) 0.34042(3) 0.12955(3) 0.0511(2) Uani 1 1 d . . . Ni1 Ni 0.05471(6) 0.37022(5) 0.11636(5) 0.0571(3) Uani 1 1 d . . . Ni2 Ni 0.29368(6) 0.36485(4) 0.34025(5) 0.0521(3) Uani 1 1 d . . . Ni3 Ni 0.36149(6) 0.54519(4) 0.15898(5) 0.0469(3) Uani 1 1 d . . . N1 N 0.0918(4) 0.4383(4) 0.1552(4) 0.063(2) Uani 1 1 d . . . N2 N 0.2184(4) 0.4192(3) 0.3158(3) 0.055(2) Uani 1 1 d . . . N3 N 0.2838(4) 0.5428(3) 0.2049(3) 0.056(2) Uani 1 1 d . . . N4 N 0.2067(7) 0.5888(5) 0.3678(5) 0.131(5) Uani 1 1 d . . . N5 N 0.0907(5) 0.6317(4) 0.1846(4) 0.086(3) Uani 1 1 d . . . N6 N -0.0181(7) 0.5025(7) 0.2888(6) 0.169(7) Uani 1 1 d . . . N7 N 0.1519(4) 0.3408(3) 0.1271(3) 0.058(2) Uani 1 1 d . . . N8 N 0.3324(3) 0.4718(3) 0.1271(3) 0.0453(17) Uani 1 1 d . . . N9 N 0.3238(4) 0.3622(3) 0.2642(3) 0.0513(19) Uani 1 1 d . . . N10 N 0.3117(5) 0.3114(4) -0.0031(4) 0.083(3) Uani 1 1 d . . . N11 N 0.3090(5) 0.2124(4) 0.1546(5) 0.092(3) Uani 1 1 d . . . N12 N 0.4946(5) 0.3440(4) 0.1406(4) 0.082(3) Uani 1 1 d . . . N13 N 0.0653(4) 0.3934(3) 0.0350(3) 0.057(2) Uani 1 1 d . . . N14 N -0.0417(4) 0.4073(3) 0.0912(3) 0.062(2) Uani 1 1 d . . . N15 N 0.0071(4) 0.2980(3) 0.0896(3) 0.0548(19) Uani 1 1 d . . . N16 N 0.0265(4) 0.3407(3) 0.1888(3) 0.061(2) Uani 1 1 d . . . N17 N 0.2564(4) 0.3538(3) 0.4155(3) 0.058(2) Uani 1 1 d . . . N18 N 0.2249(4) 0.3020(3) 0.3211(3) 0.058(2) Uani 1 1 d . . . N19 N 0.3789(4) 0.3184(3) 0.3729(3) 0.060(2) Uani 1 1 d . . . N20 N 0.3674(4) 0.4226(3) 0.3685(3) 0.0499(18) Uani 1 1 d . . . N21 N 0.4371(4) 0.5153(3) 0.2210(3) 0.0496(18) Uani 1 1 d . . . N22 N 0.4045(4) 0.6153(3) 0.1957(3) 0.0518(19) Uani 1 1 d . . . N23 N 0.4342(4) 0.5506(3) 0.1043(3) 0.0501(18) Uani 1 1 d . . . N24 N 0.3069(4) 0.5899(3) 0.0955(3) 0.0512(19) Uani 1 1 d . . . C1 C 0.1085(5) 0.4703(4) 0.1876(4) 0.055(2) Uani 1 1 d . . . C2 C 0.1858(5) 0.4541(4) 0.2973(4) 0.053(2) Uani 1 1 d . . . C3 C 0.2346(6) 0.5363(3) 0.2244(4) 0.054(2) Uani 1 1 d . . . C4 C 0.1792(7) 0.5675(5) 0.3279(5) 0.090(4) Uani 1 1 d . . . C5 C 0.1046(5) 0.5936(4) 0.2115(4) 0.065(3) Uani 1 1 d . . . C6 C 0.0365(7) 0.5097(6) 0.2778(6) 0.119(5) Uani 1 1 d . . . C7 C 0.2113(6) 0.3400(4) 0.1276(4) 0.053(2) Uani 1 1 d . . . C8 C 0.3254(4) 0.4269(4) 0.1228(3) 0.046(2) Uani 1 1 d . . . C9 C 0.3287(5) 0.3547(3) 0.2183(4) 0.050(2) Uani 1 1 d . . . C10 C 0.3137(5) 0.3223(4) 0.0427(4) 0.062(3) Uani 1 1 d . . . C11 C 0.3166(5) 0.2571(4) 0.1459(4) 0.066(3) Uani 1 1 d . . . C12 C 0.4353(6) 0.3416(4) 0.1354(4) 0.059(2) Uani 1 1 d . . . C13 C 0.1187(5) 0.3862(4) 0.0069(4) 0.059(2) Uani 1 1 d . . . H13A H 0.1587 0.3688 0.0254 0.071 Uiso 1 1 calc R . . C14 C 0.1203(5) 0.4024(4) -0.0476(4) 0.064(3) Uani 1 1 d . . . C15 C 0.0609(6) 0.4272(4) -0.0748(4) 0.061(3) Uani 1 1 d . . . C16 C 0.0051(5) 0.4348(4) -0.0462(4) 0.062(3) Uani 1 1 d . . . C17 C -0.0584(6) 0.4611(4) -0.0698(4) 0.073(3) Uani 1 1 d . . . H17A H -0.0623 0.4731 -0.1069 0.088 Uiso 1 1 calc R . . C18 C -0.1103(6) 0.4693(4) -0.0427(5) 0.072(3) Uani 1 1 d . . . H18A H -0.1505 0.4872 -0.0603 0.086 Uiso 1 1 calc R . . C19 C -0.1081(5) 0.4516(4) 0.0134(4) 0.058(2) Uani 1 1 d . . . C20 C -0.1634(6) 0.4584(4) 0.0438(5) 0.071(3) Uani 1 1 d . . . C21 C -0.1570(6) 0.4404(5) 0.0972(6) 0.085(4) Uani 1 1 d . . . C22 C -0.0941(6) 0.4139(4) 0.1191(5) 0.077(3) Uani 1 1 d . . . H22A H -0.0899 0.4004 0.1558 0.093 Uiso 1 1 calc R . . C23 C -0.0479(5) 0.4260(4) 0.0386(4) 0.060(3) Uani 1 1 d . . . C24 C 0.0088(5) 0.4178(3) 0.0079(4) 0.055(2) Uani 1 1 d . . . C25 C 0.1844(6) 0.3905(5) -0.0739(5) 0.085(3) Uani 1 1 d . . . H25A H 0.2191 0.3728 -0.0469 0.128 Uiso 1 1 calc R . . H25B H 0.2040 0.4237 -0.0858 0.128 Uiso 1 1 calc R . . H25C H 0.1719 0.3674 -0.1060 0.128 Uiso 1 1 calc R . . C26 C 0.0596(6) 0.4478(4) -0.1328(4) 0.082(3) Uani 1 1 d . . . H26A H 0.0143 0.4642 -0.1453 0.123 Uiso 1 1 calc R . . H26B H 0.0671 0.4184 -0.1576 0.123 Uiso 1 1 calc R . . H26C H 0.0965 0.4742 -0.1334 0.123 Uiso 1 1 calc R . . C27 C -0.2291(5) 0.4881(5) 0.0193(5) 0.096(4) Uani 1 1 d . . . H27A H -0.2253 0.4985 -0.0189 0.145 Uiso 1 1 calc R . . H27B H -0.2344 0.5199 0.0414 0.145 Uiso 1 1 calc R . . H27C H -0.2697 0.4651 0.0196 0.145 Uiso 1 1 calc R . . C28 C -0.2112(6) 0.4462(6) 0.1342(6) 0.114(5) Uani 1 1 d . . . H28A H -0.2518 0.4647 0.1145 0.170 Uiso 1 1 calc R . . H28B H -0.1923 0.4667 0.1670 0.170 Uiso 1 1 calc R . . H28C H -0.2254 0.4111 0.1456 0.170 Uiso 1 1 calc R . . C29 C -0.0016(5) 0.2757(4) 0.0401(4) 0.059(2) Uani 1 1 d . . . H29A H 0.0163 0.2942 0.0113 0.071 Uiso 1 1 calc R . . C30 C -0.0346(5) 0.2278(4) 0.0263(4) 0.060(3) Uani 1 1 d . . . C31 C -0.0629(5) 0.2022(4) 0.0665(5) 0.069(3) Uani 1 1 d . . . C32 C -0.0567(6) 0.2247(4) 0.1192(4) 0.073(3) Uani 1 1 d . . . C33 C -0.0850(7) 0.2018(5) 0.1643(5) 0.096(4) Uani 1 1 d . . . H33A H -0.1106 0.1697 0.1585 0.116 Uiso 1 1 calc R . . C34 C -0.0768(8) 0.2239(5) 0.2145(5) 0.108(5) Uani 1 1 d . . . H34A H -0.0960 0.2067 0.2435 0.129 Uiso 1 1 calc R . . C35 C -0.0397(6) 0.2728(5) 0.2260(4) 0.079(3) Uani 1 1 d . . . C36 C -0.0280(6) 0.2970(5) 0.2801(4) 0.078(3) Uani 1 1 d . . . C37 C 0.0132(6) 0.3403(4) 0.2860(4) 0.072(3) Uani 1 1 d . . . C38 C 0.0392(5) 0.3612(4) 0.2401(4) 0.063(3) Uani 1 1 d . . . H38A H 0.0678 0.3918 0.2455 0.076 Uiso 1 1 calc R . . C39 C -0.0111(5) 0.2952(4) 0.1836(4) 0.069(3) Uani 1 1 d . . . C40 C -0.0205(5) 0.2717(4) 0.1291(4) 0.060(3) Uani 1 1 d . . . C41 C -0.0405(5) 0.2088(4) -0.0320(4) 0.071(3) Uani 1 1 d . . . H41A H -0.0643 0.1744 -0.0352 0.106 Uiso 1 1 calc R . . H41B H 0.0061 0.2050 -0.0425 0.106 Uiso 1 1 calc R . . H41C H -0.0673 0.2344 -0.0565 0.106 Uiso 1 1 calc R . . C42 C -0.1004(7) 0.1497(5) 0.0538(5) 0.107(5) Uani 1 1 d . . . H42A H -0.0991 0.1401 0.0150 0.160 Uiso 1 1 calc R . . H42B H -0.1490 0.1531 0.0602 0.160 Uiso 1 1 calc R . . H42C H -0.0774 0.1220 0.0779 0.160 Uiso 1 1 calc R . . C43 C 0.0316(5) 0.3677(5) 0.3406(4) 0.077(3) Uani 1 1 d . . . H43A H 0.0095 0.3491 0.3688 0.116 Uiso 1 1 calc R . . H43B H 0.0149 0.4044 0.3375 0.116 Uiso 1 1 calc R . . H43C H 0.0822 0.3674 0.3511 0.116 Uiso 1 1 calc R . . C44 C -0.0595(7) 0.2743(5) 0.3264(5) 0.106(5) Uani 1 1 d . . . H44A H -0.0459 0.2955 0.3598 0.158 Uiso 1 1 calc R . . H44B H -0.0432 0.2378 0.3330 0.158 Uiso 1 1 calc R . . H44C H -0.1103 0.2745 0.3171 0.158 Uiso 1 1 calc R . . C45 C 0.2073(5) 0.2783(4) 0.2729(4) 0.067(3) Uani 1 1 d . . . H45A H 0.2293 0.2900 0.2426 0.080 Uiso 1 1 calc R . . C46 C 0.1585(5) 0.2373(4) 0.2632(4) 0.070(3) Uani 1 1 d . . . C47 C 0.1274(5) 0.2198(4) 0.3062(4) 0.068(3) Uani 1 1 d . . . C48 C 0.1447(6) 0.2452(4) 0.3583(4) 0.071(3) Uani 1 1 d . . . C49 C 0.1163(5) 0.2310(4) 0.4075(4) 0.069(3) Uani 1 1 d . . . H49A H 0.0831 0.2032 0.4055 0.083 Uiso 1 1 calc R . . C50 C 0.1348(5) 0.2558(4) 0.4568(5) 0.069(3) Uani 1 1 d . . . H50A H 0.1157 0.2442 0.4885 0.083 Uiso 1 1 calc R . . C51 C 0.1818(5) 0.2984(4) 0.4616(4) 0.059(3) Uani 1 1 d . . . C52 C 0.2003(5) 0.3258(4) 0.5106(4) 0.067(3) Uani 1 1 d . . . C53 C 0.2471(6) 0.3667(4) 0.5115(4) 0.069(3) Uani 1 1 d . . . C54 C 0.2729(5) 0.3791(4) 0.4625(4) 0.062(3) Uani 1 1 d . . . H54A H 0.3046 0.4078 0.4632 0.074 Uiso 1 1 calc R . . C55 C 0.2109(5) 0.3131(4) 0.4148(4) 0.054(2) Uani 1 1 d . . . C56 C 0.1933(5) 0.2859(4) 0.3634(4) 0.055(2) Uani 1 1 d . . . C57 C 0.1443(6) 0.2134(5) 0.2058(4) 0.085(4) Uani 1 1 d . . . H57A H 0.1092 0.1854 0.2053 0.127 Uiso 1 1 calc R . . H57B H 0.1875 0.1983 0.1959 0.127 Uiso 1 1 calc R . . H57C H 0.1272 0.2409 0.1790 0.127 Uiso 1 1 calc R . . C58 C 0.0781(6) 0.1739(5) 0.2982(5) 0.091(4) Uani 1 1 d . . . H58A H 0.0728 0.1624 0.2595 0.136 Uiso 1 1 calc R . . H58B H 0.0327 0.1846 0.3076 0.136 Uiso 1 1 calc R . . H58C H 0.0966 0.1446 0.3222 0.136 Uiso 1 1 calc R . . C59 C 0.2705(7) 0.3998(5) 0.5623(5) 0.094(4) Uani 1 1 d . . . H59A H 0.2481 0.3868 0.5932 0.142 Uiso 1 1 calc R . . H59B H 0.2575 0.4368 0.5547 0.142 Uiso 1 1 calc R . . H59C H 0.3212 0.3972 0.5718 0.142 Uiso 1 1 calc R . . C60 C 0.1687(6) 0.3107(5) 0.5609(4) 0.084(3) Uani 1 1 d . . . H60A H 0.1369 0.2807 0.5521 0.126 Uiso 1 1 calc R . . H60B H 0.1429 0.3409 0.5729 0.126 Uiso 1 1 calc R . . H60C H 0.2057 0.3005 0.5907 0.126 Uiso 1 1 calc R . . C61 C 0.3819(6) 0.2663(4) 0.3740(4) 0.071(3) Uani 1 1 d . . . H61A H 0.3428 0.2465 0.3575 0.086 Uiso 1 1 calc R . . C62 C 0.4416(7) 0.2395(4) 0.3990(5) 0.079(3) Uani 1 1 d . . . C63 C 0.4993(7) 0.2672(5) 0.4227(5) 0.083(3) Uani 1 1 d . . . C64 C 0.4954(6) 0.3233(5) 0.4216(4) 0.074(3) Uani 1 1 d . . . C65 C 0.5493(6) 0.3568(5) 0.4451(5) 0.085(3) Uani 1 1 d . . . H65A H 0.5909 0.3413 0.4634 0.102 Uiso 1 1 calc R . . C66 C 0.5445(6) 0.4107(5) 0.4426(4) 0.080(3) Uani 1 1 d . . . H66A H 0.5827 0.4317 0.4589 0.096 Uiso 1 1 calc R . . C67 C 0.4834(5) 0.4357(4) 0.4161(4) 0.060(3) Uani 1 1 d . . . C68 C 0.4751(5) 0.4917(4) 0.4111(4) 0.067(3) Uani 1 1 d . . . C69 C 0.4127(5) 0.5116(4) 0.3832(4) 0.060(3) Uani 1 1 d . . . C70 C 0.3605(5) 0.4757(4) 0.3634(4) 0.060(3) Uani 1 1 d . . . H70A H 0.3176 0.4894 0.3453 0.072 Uiso 1 1 calc R . . C71 C 0.4275(5) 0.4038(4) 0.3940(4) 0.055(2) Uani 1 1 d . . . C72 C 0.4331(5) 0.3464(4) 0.3964(4) 0.059(3) Uani 1 1 d . . . C73 C 0.4389(7) 0.1788(4) 0.3984(6) 0.104(4) Uani 1 1 d . . . H73A H 0.4830 0.1647 0.4171 0.156 Uiso 1 1 calc R . . H73B H 0.4312 0.1663 0.3600 0.156 Uiso 1 1 calc R . . H73C H 0.4006 0.1668 0.4175 0.156 Uiso 1 1 calc R . . C74 C 0.5645(7) 0.2395(5) 0.4502(5) 0.107(4) Uani 1 1 d . . . H74A H 0.5579 0.2010 0.4474 0.160 Uiso 1 1 calc R . . H74B H 0.5736 0.2497 0.4893 0.160 Uiso 1 1 calc R . . H74C H 0.6042 0.2498 0.4318 0.160 Uiso 1 1 calc R . . C75 C 0.5304(6) 0.5302(4) 0.4347(5) 0.087(4) Uani 1 1 d . . . H75A H 0.5139 0.5665 0.4268 0.130 Uiso 1 1 calc R . . H75B H 0.5727 0.5241 0.4180 0.130 Uiso 1 1 calc R . . H75C H 0.5406 0.5251 0.4749 0.130 Uiso 1 1 calc R . . C76 C 0.3988(6) 0.5700(4) 0.3744(5) 0.081(3) Uani 1 1 d . . . H76A H 0.3521 0.5750 0.3539 0.121 Uiso 1 1 calc R . . H76B H 0.4334 0.5850 0.3532 0.121 Uiso 1 1 calc R . . H76C H 0.4021 0.5878 0.4103 0.121 Uiso 1 1 calc R . . C77 C 0.4980(5) 0.5318(3) 0.1085(4) 0.054(2) Uani 1 1 d . . . H77A H 0.5141 0.5120 0.1409 0.065 Uiso 1 1 calc R . . C78 C 0.5434(5) 0.5381(4) 0.0708(5) 0.063(3) Uani 1 1 d . . . C79 C 0.5200(6) 0.5649(4) 0.0232(5) 0.068(3) Uani 1 1 d . . . C80 C 0.4519(5) 0.5863(4) 0.0159(4) 0.059(3) Uani 1 1 d . . . C81 C 0.4228(7) 0.6167(4) -0.0312(5) 0.073(3) Uani 1 1 d . . . H81A H 0.4488 0.6214 -0.0611 0.087 Uiso 1 1 calc R . . C82 C 0.3599(7) 0.6385(4) -0.0337(4) 0.077(3) Uani 1 1 d . . . H82A H 0.3429 0.6593 -0.0651 0.093 Uiso 1 1 calc R . . C83 C 0.3168(6) 0.6319(4) 0.0087(4) 0.061(3) Uani 1 1 d . . . C84 C 0.2503(6) 0.6559(4) 0.0084(5) 0.070(3) Uani 1 1 d . . . C85 C 0.2140(5) 0.6452(4) 0.0515(5) 0.067(3) Uani 1 1 d . . . C86 C 0.2443(5) 0.6123(3) 0.0945(4) 0.057(2) Uani 1 1 d . . . H86A H 0.2190 0.6055 0.1244 0.069 Uiso 1 1 calc R . . C87 C 0.3432(5) 0.6007(3) 0.0538(4) 0.052(2) Uani 1 1 d . . . C88 C 0.4119(5) 0.5788(3) 0.0576(4) 0.051(2) Uani 1 1 d . . . C89 C 0.6159(5) 0.5168(4) 0.0847(5) 0.083(3) Uani 1 1 d . . . H89A H 0.6422 0.5239 0.0540 0.124 Uiso 1 1 calc R . . H89B H 0.6138 0.4784 0.0908 0.124 Uiso 1 1 calc R . . H89C H 0.6390 0.5340 0.1183 0.124 Uiso 1 1 calc R . . C90 C 0.5678(6) 0.5722(4) -0.0201(5) 0.086(4) Uani 1 1 d . . . H90A H 0.5434 0.5921 -0.0515 0.128 Uiso 1 1 calc R . . H90B H 0.5815 0.5374 -0.0328 0.128 Uiso 1 1 calc R . . H90C H 0.6094 0.5917 -0.0041 0.128 Uiso 1 1 calc R . . C91 C 0.2187(7) 0.6908(5) -0.0378(5) 0.099(4) Uani 1 1 d . . . H91A H 0.2511 0.6944 -0.0649 0.149 Uiso 1 1 calc R . . H91B H 0.2092 0.7258 -0.0231 0.149 Uiso 1 1 calc R . . H91C H 0.1751 0.6750 -0.0556 0.149 Uiso 1 1 calc R . . C92 C 0.1469(6) 0.6707(4) 0.0587(5) 0.083(3) Uani 1 1 d . . . H92A H 0.1309 0.6929 0.0265 0.125 Uiso 1 1 calc R . . H92B H 0.1534 0.6928 0.0921 0.125 Uiso 1 1 calc R . . H92C H 0.1120 0.6434 0.0624 0.125 Uiso 1 1 calc R . . C93 C 0.4517(4) 0.4655(3) 0.2343(4) 0.050(2) Uani 1 1 d . . . H93A H 0.4197 0.4390 0.2192 0.060 Uiso 1 1 calc R . . C94 C 0.5112(5) 0.4491(3) 0.2691(4) 0.054(2) Uani 1 1 d . . . C95 C 0.5602(5) 0.4878(3) 0.2906(4) 0.057(2) Uani 1 1 d . . . C96 C 0.5439(5) 0.5412(3) 0.2788(4) 0.060(3) Uani 1 1 d . . . C97 C 0.5871(6) 0.5844(4) 0.2998(4) 0.068(3) Uani 1 1 d . . . H97A H 0.6297 0.5773 0.3229 0.081 Uiso 1 1 calc R . . C98 C 0.5689(6) 0.6354(4) 0.2876(4) 0.072(3) Uani 1 1 d . . . H98A H 0.5988 0.6632 0.3028 0.087 Uiso 1 1 calc R . . C99 C 0.5060(5) 0.6483(3) 0.2526(4) 0.058(2) Uani 1 1 d . . . C100 C 0.4850(6) 0.7015(4) 0.2378(4) 0.073(3) Uani 1 1 d . . . C101 C 0.4240(6) 0.7088(3) 0.2043(4) 0.063(3) Uani 1 1 d . . . C102 C 0.3856(5) 0.6653(3) 0.1836(4) 0.061(3) Uani 1 1 d . . . H10A H 0.3435 0.6713 0.1594 0.073 Uiso 1 1 calc R . . C103 C 0.4639(5) 0.6071(3) 0.2296(4) 0.051(2) Uani 1 1 d . . . C104 C 0.4825(5) 0.5529(3) 0.2445(4) 0.048(2) Uani 1 1 d . . . C105 C 0.5232(5) 0.3909(3) 0.2798(4) 0.065(3) Uani 1 1 d . . . H10B H 0.4832 0.3708 0.2613 0.097 Uiso 1 1 calc R . . H10C H 0.5285 0.3841 0.3197 0.097 Uiso 1 1 calc R . . H10D H 0.5655 0.3797 0.2653 0.097 Uiso 1 1 calc R . . C106 C 0.6265(5) 0.4711(4) 0.3254(5) 0.077(3) Uani 1 1 d . . . H10E H 0.6277 0.4324 0.3286 0.115 Uiso 1 1 calc R . . H10F H 0.6289 0.4867 0.3624 0.115 Uiso 1 1 calc R . . H10G H 0.6664 0.4832 0.3082 0.115 Uiso 1 1 calc R . . C107 C 0.3955(6) 0.7629(4) 0.1883(5) 0.081(3) Uani 1 1 d . . . H10H H 0.4277 0.7900 0.2055 0.121 Uiso 1 1 calc R . . H10I H 0.3501 0.7673 0.2010 0.121 Uiso 1 1 calc R . . H10J H 0.3900 0.7667 0.1480 0.121 Uiso 1 1 calc R . . C108 C 0.5298(7) 0.7475(4) 0.2596(5) 0.097(4) Uani 1 1 d . . . H10K H 0.5078 0.7807 0.2455 0.146 Uiso 1 1 calc R . . H10L H 0.5757 0.7443 0.2475 0.146 Uiso 1 1 calc R . . H10M H 0.5352 0.7476 0.3001 0.146 Uiso 1 1 calc R . . O10 O -0.2919(9) 0.1736(8) 0.0592(9) 0.263(9) Uani 1 1 d U . . O4 O 0.351(3) 0.7117(14) -0.1585(17) 0.68(4) Uani 1 1 d DU . . O1 O 0.7073(11) 0.4759(6) 0.5099(6) 0.214(7) Uani 1 1 d DU . . C110 C 0.469(2) 0.2976(13) 0.5679(13) 0.211(17) Uani 1 1 d . . . O2 O 0.0590(19) 0.4191(15) 0.526(2) 0.56(3) Uani 1 1 d DU . . N25 N 0.4119(13) 0.3040(14) 0.5417(10) 0.261(14) Uani 1 1 d . . . O5 O 0.2624(13) 0.7997(8) 0.0524(13) 0.355(17) Uani 1 1 d DU . . O13 O 0.2307(9) 0.7161(9) 0.2030(13) 0.328(14) Uani 1 1 d U . . C115 C 0.2491(15) 0.8360(14) 0.0925(13) 0.271(16) Uani 1 1 d DU . . C112 C 0.0690(17) 0.4336(16) 0.4724(13) 0.31(3) Uani 1 1 d DU . . C113 C -0.243(2) 0.5687(16) 0.1961(13) 0.30(2) Uani 1 1 d DU . . O12 O 0.2668(18) 0.6855(15) 0.2792(15) 0.44(2) Uani 1 1 d U . . O3 O -0.2837(19) 0.6146(16) 0.1950(19) 0.53(3) Uani 1 1 d DU . . O7 O -0.1616(13) 0.465(2) 0.2912(14) 0.56(3) Uani 1 1 d U . . O15 O -0.084(3) 0.0429(19) -0.0764(12) 0.82(6) Uani 1 1 d . . . O9 O -0.229(2) 0.339(2) 0.226(2) 0.72(4) Uani 1 1 d U . . O6 O -0.113(3) 0.5701(19) 0.330(3) 0.79(4) Uani 1 1 d U . . O8 O -0.369(5) 0.219(3) 0.110(3) 0.78(5) Uani 1 1 d U . . O11 O 0.166(3) 0.4963(12) 0.4495(15) 0.57(3) Uani 1 1 d U . . C111 C 0.7216(18) 0.4216(11) 0.5094(17) 0.46(3) Uani 1 1 d DU . . C109 C 0.5332(18) 0.2997(10) 0.5871(14) 0.197(12) Uani 1 1 d U . . C114 C 0.3612(9) 0.6591(15) -0.1757(8) 0.243(16) Uani 1 1 d DU . . O14 O 0.755(2) 0.610(2) 0.281(2) 0.62(3) Uani 1 1 d U . . 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 0.0601(6) 0.0657(6) 0.0617(6) 0.0056(4) 0.0125(4) 0.0089(4) Mo2 0.0578(5) 0.0396(4) 0.0570(5) -0.0012(4) 0.0113(4) -0.0012(4) Ni1 0.0536(7) 0.0644(8) 0.0534(7) 0.0087(6) 0.0079(6) -0.0048(6) Ni2 0.0566(7) 0.0456(7) 0.0537(7) 0.0074(6) 0.0071(6) -0.0072(6) Ni3 0.0500(7) 0.0353(6) 0.0553(7) -0.0001(5) 0.0067(5) 0.0002(5) N1 0.055(5) 0.073(6) 0.060(6) 0.017(5) 0.005(4) -0.002(4) N2 0.058(5) 0.060(5) 0.046(5) 0.012(4) 0.006(4) 0.000(4) N3 0.065(5) 0.042(4) 0.059(5) -0.002(4) 0.005(4) 0.007(4) N4 0.131(10) 0.154(12) 0.105(10) -0.047(9) 0.004(8) 0.050(9) N5 0.087(7) 0.088(7) 0.081(7) 0.003(6) 0.008(5) 0.036(6) N6 0.107(10) 0.233(17) 0.185(14) 0.067(13) 0.087(10) 0.043(11) N7 0.063(5) 0.065(5) 0.046(5) 0.013(4) 0.009(4) -0.007(4) N8 0.038(4) 0.042(4) 0.057(5) 0.001(4) 0.011(3) -0.002(3) N9 0.057(5) 0.041(4) 0.056(5) 0.008(4) 0.009(4) -0.006(3) N10 0.076(6) 0.105(8) 0.068(6) -0.017(6) 0.009(5) -0.002(5) N11 0.084(7) 0.048(6) 0.135(9) 0.011(6) -0.019(6) 0.000(5) N12 0.067(6) 0.103(8) 0.074(6) 0.012(5) 0.005(5) 0.007(6) N13 0.054(5) 0.055(5) 0.064(5) 0.010(4) 0.008(4) -0.003(4) N14 0.057(5) 0.071(6) 0.060(5) 0.004(4) 0.015(4) -0.003(4) N15 0.048(5) 0.062(5) 0.055(5) 0.008(4) 0.010(4) -0.003(4) N16 0.048(5) 0.070(5) 0.064(6) -0.004(4) 0.005(4) -0.013(4) N17 0.069(5) 0.061(5) 0.042(5) 0.010(4) 0.007(4) -0.005(4) N18 0.063(5) 0.060(5) 0.049(5) 0.004(4) 0.003(4) -0.017(4) N19 0.070(6) 0.044(5) 0.065(5) 0.011(4) 0.006(4) 0.002(4) N20 0.062(5) 0.039(4) 0.048(4) 0.002(3) 0.003(4) -0.004(4) N21 0.051(4) 0.043(4) 0.053(5) -0.001(3) -0.002(4) -0.002(4) N22 0.063(5) 0.034(4) 0.057(5) 0.000(3) 0.004(4) -0.001(4) N23 0.050(5) 0.042(4) 0.061(5) -0.001(4) 0.018(4) -0.006(4) N24 0.054(5) 0.032(4) 0.065(5) -0.003(4) 0.001(4) 0.000(3) C1 0.048(6) 0.059(6) 0.058(6) 0.016(5) 0.008(5) 0.003(5) C2 0.059(6) 0.061(6) 0.041(5) -0.001(5) 0.009(5) -0.009(5) C3 0.069(7) 0.041(5) 0.050(6) 0.004(4) 0.006(5) 0.006(5) C4 0.107(10) 0.090(9) 0.073(8) -0.018(7) 0.007(7) 0.042(8) C5 0.063(7) 0.063(7) 0.066(7) -0.004(6) 0.003(5) 0.025(5) C6 0.086(10) 0.142(13) 0.144(13) 0.045(10) 0.068(10) 0.029(9) C7 0.068(7) 0.049(5) 0.041(5) 0.012(4) 0.005(5) 0.002(5) C8 0.041(5) 0.051(6) 0.046(5) 0.004(4) 0.008(4) 0.007(4) C9 0.051(6) 0.036(5) 0.058(6) 0.006(4) -0.003(5) -0.004(4) C10 0.071(7) 0.058(6) 0.058(7) -0.004(5) 0.014(5) 0.000(5) C11 0.066(7) 0.061(7) 0.068(7) -0.002(5) -0.007(5) -0.002(5) C12 0.069(7) 0.050(6) 0.060(6) 0.010(5) 0.017(5) 0.006(5) C13 0.054(6) 0.070(7) 0.053(6) 0.009(5) 0.008(5) 0.001(5) C14 0.070(7) 0.067(7) 0.055(6) 0.007(5) 0.012(5) 0.001(5) C15 0.081(7) 0.056(6) 0.047(6) 0.005(5) 0.013(5) -0.003(5) C16 0.071(7) 0.052(6) 0.057(7) 0.009(5) -0.010(6) -0.001(5) C17 0.097(9) 0.064(7) 0.054(7) 0.004(5) -0.006(6) 0.008(6) C18 0.074(8) 0.063(7) 0.074(8) -0.001(6) -0.007(6) 0.004(6) C19 0.049(6) 0.056(6) 0.067(7) -0.007(5) -0.002(5) 0.003(5) C20 0.068(7) 0.070(7) 0.075(8) -0.015(6) 0.007(6) -0.012(6) C21 0.063(8) 0.097(9) 0.103(10) -0.012(8) 0.035(7) -0.002(7) C22 0.072(8) 0.084(8) 0.081(8) -0.001(6) 0.026(7) -0.015(6) C23 0.054(6) 0.064(6) 0.060(7) -0.004(5) 0.004(5) 0.002(5) C24 0.063(6) 0.043(5) 0.059(6) -0.002(5) 0.007(5) 0.007(5) C25 0.097(9) 0.097(9) 0.067(7) 0.008(6) 0.029(7) -0.008(7) C26 0.108(9) 0.063(7) 0.077(8) 0.018(6) 0.024(7) 0.007(6) C27 0.046(6) 0.124(11) 0.115(10) -0.029(8) -0.004(6) 0.017(7) C28 0.076(9) 0.126(12) 0.147(13) -0.016(10) 0.043(9) -0.007(8) C29 0.053(6) 0.074(7) 0.050(6) 0.000(5) 0.008(5) 0.004(5) C30 0.060(6) 0.063(7) 0.056(6) 0.000(5) 0.006(5) 0.001(5) C31 0.070(7) 0.071(7) 0.066(7) -0.006(6) 0.005(6) -0.013(6) C32 0.083(8) 0.075(7) 0.060(7) 0.011(6) 0.008(6) -0.026(6) C33 0.128(11) 0.091(9) 0.067(8) 0.005(7) 0.005(7) -0.063(8) C34 0.163(13) 0.104(10) 0.057(8) 0.005(7) 0.021(8) -0.080(9) C35 0.090(8) 0.093(8) 0.055(7) 0.012(6) 0.015(6) -0.034(7) C36 0.076(7) 0.094(9) 0.066(7) 0.007(6) 0.019(6) -0.032(7) C37 0.079(7) 0.087(8) 0.054(7) 0.004(6) 0.017(6) -0.027(6) C38 0.063(6) 0.064(6) 0.061(7) 0.001(5) 0.004(5) -0.017(5) C39 0.073(7) 0.071(7) 0.062(7) 0.010(6) 0.011(6) -0.017(6) C40 0.053(6) 0.074(7) 0.052(6) 0.010(5) 0.007(5) -0.014(5) C41 0.082(8) 0.064(7) 0.067(7) -0.002(5) 0.017(6) -0.006(6) C42 0.136(12) 0.096(10) 0.090(9) -0.008(7) 0.021(8) -0.057(9) C43 0.071(7) 0.105(9) 0.057(7) 0.011(6) 0.013(6) -0.021(6) C44 0.139(12) 0.120(11) 0.059(7) 0.011(7) 0.021(7) -0.061(9) C45 0.081(7) 0.058(6) 0.060(7) 0.010(5) 0.007(6) -0.024(6) C46 0.076(7) 0.077(7) 0.056(6) 0.010(5) 0.012(5) -0.028(6) C47 0.075(7) 0.059(6) 0.068(7) 0.005(5) 0.001(6) -0.025(5) C48 0.079(7) 0.075(7) 0.061(7) 0.010(6) 0.013(6) -0.023(6) C49 0.065(7) 0.067(7) 0.074(8) 0.013(6) 0.006(6) -0.013(5) C50 0.069(7) 0.073(7) 0.065(7) 0.020(6) 0.004(6) -0.018(6) C51 0.043(5) 0.078(7) 0.051(6) 0.016(5) -0.008(5) 0.002(5) C52 0.064(7) 0.086(8) 0.046(6) 0.024(5) -0.005(5) -0.006(6) C53 0.079(7) 0.076(7) 0.048(6) 0.002(5) -0.002(5) -0.009(6) C54 0.072(7) 0.058(6) 0.052(6) 0.015(5) -0.001(5) -0.014(5) C55 0.056(6) 0.053(6) 0.054(6) 0.017(5) 0.009(5) -0.001(5) C56 0.060(6) 0.058(6) 0.046(6) 0.007(5) 0.004(5) -0.010(5) C57 0.098(9) 0.093(9) 0.063(7) -0.004(6) 0.012(6) -0.046(7) C58 0.089(8) 0.107(10) 0.076(8) -0.002(7) 0.014(7) -0.046(7) C59 0.108(10) 0.102(9) 0.070(8) -0.004(7) 0.001(7) -0.035(8) C60 0.082(8) 0.119(10) 0.051(6) 0.010(6) 0.009(6) -0.024(7) C61 0.081(8) 0.053(7) 0.080(8) 0.014(6) 0.011(6) -0.005(6) C62 0.089(9) 0.054(7) 0.094(9) 0.028(6) 0.018(7) 0.014(6) C63 0.084(9) 0.079(8) 0.086(8) 0.031(7) 0.010(7) 0.027(7) C64 0.079(8) 0.071(8) 0.068(7) 0.015(6) -0.001(6) 0.000(6) C65 0.076(8) 0.080(9) 0.092(9) 0.016(7) -0.012(7) 0.016(7) C66 0.061(7) 0.095(9) 0.078(8) 0.001(7) -0.014(6) -0.016(6) C67 0.060(6) 0.062(7) 0.053(6) 0.002(5) -0.007(5) 0.000(5) C68 0.063(7) 0.076(8) 0.063(7) -0.009(6) 0.011(5) -0.020(6) C69 0.068(7) 0.048(6) 0.065(7) -0.011(5) 0.018(5) -0.007(5) C70 0.068(7) 0.050(6) 0.063(6) 0.000(5) 0.012(5) -0.006(5) C71 0.054(6) 0.059(6) 0.049(6) 0.002(5) 0.001(5) -0.004(5) C72 0.066(7) 0.053(6) 0.058(6) 0.017(5) 0.007(5) 0.003(5) C73 0.115(10) 0.054(7) 0.147(12) 0.024(7) 0.032(9) 0.021(7) C74 0.124(11) 0.074(8) 0.113(10) 0.023(7) -0.016(9) 0.025(8) C75 0.101(9) 0.079(8) 0.077(8) -0.021(6) 0.000(7) -0.027(7) C76 0.098(9) 0.048(6) 0.098(9) 0.001(6) 0.023(7) -0.006(6) C77 0.056(6) 0.044(5) 0.063(6) -0.009(4) 0.013(5) -0.004(5) C78 0.059(6) 0.052(6) 0.085(8) -0.017(6) 0.031(6) -0.017(5) C79 0.082(8) 0.052(6) 0.076(8) -0.016(6) 0.029(6) -0.022(6) C80 0.074(7) 0.038(5) 0.070(7) -0.007(5) 0.022(6) -0.021(5) C81 0.100(9) 0.050(6) 0.073(8) -0.009(6) 0.028(7) -0.018(6) C82 0.123(11) 0.055(7) 0.052(7) 0.008(5) 0.006(7) -0.010(7) C83 0.079(7) 0.045(6) 0.059(6) 0.005(5) 0.007(6) -0.008(5) C84 0.073(7) 0.056(6) 0.074(7) 0.014(6) -0.007(6) -0.001(6) C85 0.058(7) 0.048(6) 0.087(8) 0.002(5) -0.013(6) 0.006(5) C86 0.057(6) 0.044(5) 0.067(7) -0.004(5) -0.006(5) 0.000(5) C87 0.060(6) 0.047(5) 0.052(6) 0.009(5) 0.012(5) -0.012(5) C88 0.059(6) 0.045(5) 0.051(6) -0.010(4) 0.012(5) -0.017(5) C89 0.064(7) 0.069(7) 0.121(10) -0.023(7) 0.035(7) -0.003(6) C90 0.095(9) 0.073(8) 0.100(9) -0.011(6) 0.057(7) -0.019(6) C91 0.111(10) 0.076(8) 0.099(9) 0.027(7) -0.027(8) 0.012(7) C92 0.073(8) 0.071(7) 0.097(9) -0.005(6) -0.015(6) 0.011(6) C93 0.049(5) 0.037(5) 0.063(6) 0.005(4) 0.006(5) 0.005(4) C94 0.066(6) 0.037(5) 0.057(6) 0.000(4) 0.001(5) 0.006(5) C95 0.072(7) 0.036(5) 0.062(6) 0.004(4) 0.008(5) 0.007(5) C96 0.077(7) 0.039(5) 0.062(6) -0.007(5) 0.004(5) -0.008(5) C97 0.085(7) 0.042(6) 0.069(7) -0.007(5) -0.011(6) -0.010(5) C98 0.100(9) 0.044(6) 0.067(7) -0.002(5) -0.009(6) -0.015(6) C99 0.071(7) 0.037(5) 0.061(6) 0.001(4) -0.007(5) -0.006(5) C100 0.101(9) 0.035(5) 0.077(7) -0.013(5) -0.009(7) -0.011(5) C101 0.079(7) 0.034(5) 0.072(7) -0.005(5) -0.004(6) -0.002(5) C102 0.075(7) 0.038(5) 0.069(7) 0.006(5) 0.005(5) 0.012(5) C103 0.061(6) 0.033(5) 0.057(6) -0.005(4) 0.008(5) -0.008(4) C104 0.054(6) 0.034(5) 0.058(6) 0.002(4) 0.009(5) -0.002(4) C105 0.074(7) 0.034(5) 0.084(7) 0.008(5) 0.005(6) 0.003(5) C106 0.075(7) 0.051(6) 0.094(8) 0.009(6) -0.021(6) -0.004(5) C107 0.094(8) 0.048(6) 0.092(8) -0.004(6) -0.017(7) -0.007(6) C108 0.120(10) 0.045(6) 0.113(10) 0.001(6) -0.026(8) -0.008(7) O10 0.223(17) 0.239(18) 0.32(2) 0.122(17) 0.016(15) -0.016(14) O4 0.75(7) 0.83(8) 0.43(5) 0.41(6) 0.03(5) 0.05(7) O1 0.33(2) 0.144(12) 0.169(13) -0.007(10) 0.051(14) -0.016(14) C110 0.28(4) 0.20(3) 0.16(3) 0.08(2) 0.07(3) 0.09(4) O2 0.28(3) 0.36(4) 1.05(8) -0.04(5) 0.14(5) -0.11(3) N25 0.19(2) 0.44(4) 0.16(2) 0.02(2) 0.038(16) 0.06(2) O5 0.25(2) 0.181(19) 0.58(5) -0.06(2) -0.14(3) 0.013(16) O13 0.158(14) 0.31(2) 0.55(4) -0.21(3) 0.17(2) -0.038(15) C115 0.16(2) 0.25(4) 0.38(4) 0.01(3) -0.04(3) 0.07(2) C112 0.21(3) 0.41(5) 0.28(3) -0.27(4) -0.09(3) 0.12(3) C113 0.32(4) 0.39(5) 0.20(3) 0.05(3) 0.05(3) 0.15(3) O12 0.42(4) 0.47(4) 0.46(4) 0.09(4) 0.13(3) 0.03(3) O3 0.34(4) 0.65(6) 0.63(6) -0.30(5) 0.16(4) -0.02(4) O7 0.21(2) 1.01(8) 0.44(4) -0.06(5) -0.01(2) -0.14(4) O15 1.42(14) 0.81(8) 0.26(3) -0.07(4) 0.30(5) -0.71(10) O9 0.64(6) 0.75(7) 0.75(7) 0.41(5) 0.01(5) -0.33(5) O6 0.96(8) 0.54(5) 0.97(8) 0.25(5) 0.48(7) 0.51(6) O8 1.06(10) 0.65(8) 0.62(7) -0.09(6) 0.10(7) 0.09(7) O11 1.02(7) 0.33(3) 0.46(4) 0.20(3) 0.52(5) 0.29(4) C111 0.23(3) 0.58(7) 0.53(6) -0.38(5) -0.10(4) -0.03(4) C109 0.24(3) 0.106(15) 0.23(3) 0.004(16) 0.01(3) 0.01(2) C114 0.077(11) 0.56(5) 0.096(13) 0.09(2) 0.020(9) 0.091(19) O14 0.52(6) 0.61(6) 0.78(7) -0.17(6) 0.27(5) -0.28(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 C4 2.117(13) . ? Mo1 C5 2.125(11) . ? Mo1 C6 2.141(14) . ? Mo1 C3 2.150(11) . ? Mo1 C2 2.167(11) . ? Mo1 C1 2.176(12) . ? Mo2 C11 2.145(11) . ? Mo2 C10 2.153(11) . ? Mo2 C7 2.155(11) . ? Mo2 C12 2.166(11) . ? Mo2 C9 2.183(10) . ? Mo2 C8 2.190(9) . ? Ni1 N7 2.008(9) . ? Ni1 N1 2.044(10) . ? Ni1 N16 2.064(8) . ? Ni1 N14 2.103(8) . ? Ni1 N15 2.104(8) . ? Ni1 N13 2.108(8) . ? Ni2 N9 2.026(8) . ? Ni2 N2 2.031(8) . ? Ni2 N18 2.082(7) . ? Ni2 N17 2.086(7) . ? Ni2 N20 2.089(7) . ? Ni2 N19 2.091(8) . ? Ni3 N3 2.002(9) . ? Ni3 N8 2.056(7) . ? Ni3 N23 2.079(7) . ? Ni3 N24 2.082(7) . ? Ni3 N21 2.093(7) . ? Ni3 N22 2.103(7) . ? N1 C1 1.144(11) . ? N2 C2 1.138(11) . ? N3 C3 1.137(11) . ? N4 C4 1.171(14) . ? N5 C5 1.174(12) . ? N6 C6 1.142(15) . ? N7 C7 1.151(11) . ? N8 C8 1.145(10) . ? N9 C9 1.154(10) . ? N10 C10 1.146(11) . ? N11 C11 1.164(12) . ? N12 C12 1.141(12) . ? N13 C13 1.333(11) . ? N13 C24 1.347(11) . ? N14 C22 1.312(12) . ? N14 C23 1.359(12) . ? N15 C29 1.322(11) . ? N15 C40 1.344(11) . ? N16 C38 1.345(12) . ? N16 C39 1.355(12) . ? N17 C54 1.313(11) . ? N17 C55 1.353(11) . ? N18 C45 1.323(11) . ? N18 C56 1.336(11) . ? N19 C61 1.315(12) . ? N19 C72 1.327(12) . ? N20 C71 1.329(11) . ? N20 C70 1.352(11) . ? N21 C93 1.319(10) . ? N21 C104 1.366(10) . ? N22 C102 1.336(10) . ? N22 C103 1.336(11) . ? N23 C77 1.316(11) . ? N23 C88 1.360(11) . ? N24 C86 1.336(11) . ? N24 C87 1.346(11) . ? C13 C14 1.396(13) . ? C14 C15 1.394(13) . ? C14 C25 1.508(14) . ? C15 C16 1.383(14) . ? C15 C26 1.506(13) . ? C16 C24 1.381(13) . ? C16 C17 1.446(14) . ? C17 C18 1.297(14) . ? C18 C19 1.436(14) . ? C19 C23 1.397(13) . ? C19 C20 1.399(14) . ? C20 C21 1.370(15) . ? C20 C27 1.525(14) . ? C21 C22 1.429(16) . ? C21 C28 1.488(16) . ? C23 C24 1.430(13) . ? C29 C30 1.386(13) . ? C30 C31 1.354(13) . ? C30 C41 1.493(13) . ? C31 C32 1.397(14) . ? C31 C42 1.522(14) . ? C32 C40 1.383(13) . ? C32 C33 1.421(14) . ? C33 C34 1.335(15) . ? C34 C35 1.436(15) . ? C35 C39 1.366(13) . ? C35 C36 1.446(14) . ? C36 C37 1.348(14) . ? C36 C44 1.474(14) . ? C37 C38 1.395(13) . ? C37 C43 1.500(14) . ? C39 C40 1.444(14) . ? C45 C46 1.400(13) . ? C46 C47 1.357(13) . ? C46 C57 1.516(14) . ? C47 C48 1.421(14) . ? C47 C58 1.497(13) . ? C48 C56 1.388(13) . ? C48 C49 1.437(13) . ? C49 C50 1.360(14) . ? C50 C51 1.403(13) . ? C51 C52 1.384(13) . ? C51 C55 1.395(12) . ? C52 C53 1.372(14) . ? C52 C60 1.498(13) . ? C53 C54 1.397(13) . ? C53 C59 1.512(14) . ? C55 C56 1.429(12) . ? C61 C62 1.404(15) . ? C62 C63 1.377(16) . ? C62 C73 1.531(15) . ? C63 C64 1.417(15) . ? C63 C74 1.517(15) . ? C64 C65 1.402(15) . ? C64 C72 1.404(14) . ? C65 C66 1.364(15) . ? C66 C67 1.418(14) . ? C67 C71 1.396(13) . ? C67 C68 1.424(14) . ? C68 C69 1.396(14) . ? C68 C75 1.500(13) . ? C69 C70 1.393(13) . ? C69 C76 1.506(13) . ? C71 C72 1.453(13) . ? C77 C78 1.373(13) . ? C78 C79 1.366(14) . ? C78 C89 1.498(14) . ? C79 C80 1.415(14) . ? C79 C90 1.513(13) . ? C80 C88 1.377(12) . ? C80 C81 1.430(14) . ? C81 C82 1.331(15) . ? C82 C83 1.429(14) . ? C83 C87 1.391(12) . ? C83 C84 1.425(14) . ? C84 C85 1.373(14) . ? C84 C91 1.492(14) . ? C85 C86 1.402(13) . ? C85 C92 1.486(14) . ? C87 C88 1.434(12) . ? C93 C94 1.395(12) . ? C94 C95 1.410(12) . ? C94 C105 1.506(11) . ? C95 C96 1.406(12) . ? C95 C106 1.499(13) . ? C96 C104 1.388(12) . ? C96 C97 1.424(12) . ? C97 C98 1.357(13) . ? C98 C99 1.425(13) . ? C99 C103 1.389(12) . ? C99 C100 1.435(13) . ? C100 C101 1.351(13) . ? C100 C108 1.502(13) . ? C101 C102 1.381(13) . ? C101 C107 1.506(13) . ? C103 C104 1.447(11) . ? O4 C114 1.41(2) . ? O1 C111 1.40(2) . ? C110 N25 1.21(4) . ? C110 C109 1.26(4) . ? O2 C112 1.41(2) . ? O5 C115 1.392(18) . ? C113 O3 1.399(19) . ? 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 C4 Mo1 C5 92.9(4) . . ? C4 Mo1 C6 98.0(6) . . ? C5 Mo1 C6 92.3(5) . . ? C4 Mo1 C3 89.0(4) . . ? C5 Mo1 C3 84.8(4) . . ? C6 Mo1 C3 172.6(5) . . ? C4 Mo1 C2 87.6(4) . . ? C5 Mo1 C2 171.9(4) . . ? C6 Mo1 C2 95.6(4) . . ? C3 Mo1 C2 87.1(3) . . ? C4 Mo1 C1 171.1(4) . . ? C5 Mo1 C1 94.9(4) . . ? C6 Mo1 C1 86.0(5) . . ? C3 Mo1 C1 87.5(3) . . ? C2 Mo1 C1 84.1(3) . . ? C11 Mo2 C10 88.6(4) . . ? C11 Mo2 C7 85.3(4) . . ? C10 Mo2 C7 92.0(4) . . ? C11 Mo2 C12 94.8(4) . . ? C10 Mo2 C12 90.5(4) . . ? C7 Mo2 C12 177.4(4) . . ? C11 Mo2 C9 88.5(3) . . ? C10 Mo2 C9 176.7(3) . . ? C7 Mo2 C9 86.2(3) . . ? C12 Mo2 C9 91.2(3) . . ? C11 Mo2 C8 173.1(4) . . ? C10 Mo2 C8 97.9(3) . . ? C7 Mo2 C8 92.1(3) . . ? C12 Mo2 C8 87.5(3) . . ? C9 Mo2 C8 84.9(3) . . ? N7 Ni1 N1 89.3(3) . . ? N7 Ni1 N16 96.4(3) . . ? N1 Ni1 N16 91.4(3) . . ? N7 Ni1 N14 169.1(3) . . ? N1 Ni1 N14 90.1(3) . . ? N16 Ni1 N14 94.5(3) . . ? N7 Ni1 N15 94.7(3) . . ? N1 Ni1 N15 169.2(3) . . ? N16 Ni1 N15 78.2(3) . . ? N14 Ni1 N15 87.8(3) . . ? N7 Ni1 N13 90.6(3) . . ? N1 Ni1 N13 97.5(3) . . ? N16 Ni1 N13 168.8(3) . . ? N14 Ni1 N13 78.6(3) . . ? N15 Ni1 N13 92.5(3) . . ? N9 Ni2 N2 92.4(3) . . ? N9 Ni2 N18 91.6(3) . . ? N2 Ni2 N18 92.2(3) . . ? N9 Ni2 N17 169.8(3) . . ? N2 Ni2 N17 91.4(3) . . ? N18 Ni2 N17 78.7(3) . . ? N9 Ni2 N20 93.0(3) . . ? N2 Ni2 N20 93.2(3) . . ? N18 Ni2 N20 172.8(3) . . ? N17 Ni2 N20 96.2(3) . . ? N9 Ni2 N19 91.0(3) . . ? N2 Ni2 N19 171.0(3) . . ? N18 Ni2 N19 96.0(3) . . ? N17 Ni2 N19 86.7(3) . . ? N20 Ni2 N19 78.3(3) . . ? N3 Ni3 N8 89.9(3) . . ? N3 Ni3 N23 173.7(3) . . ? N8 Ni3 N23 89.4(3) . . ? N3 Ni3 N24 95.1(3) . . ? N8 Ni3 N24 97.0(3) . . ? N23 Ni3 N24 78.8(3) . . ? N3 Ni3 N21 95.2(3) . . ? N8 Ni3 N21 94.3(3) . . ? N23 Ni3 N21 91.1(3) . . ? N24 Ni3 N21 164.7(3) . . ? N3 Ni3 N22 94.1(3) . . ? N8 Ni3 N22 172.1(3) . . ? N23 Ni3 N22 87.4(3) . . ? N24 Ni3 N22 89.5(3) . . ? N21 Ni3 N22 78.5(3) . . ? C1 N1 Ni1 163.8(8) . . ? C2 N2 Ni2 166.9(8) . . ? C3 N3 Ni3 169.1(8) . . ? C7 N7 Ni1 158.0(8) . . ? C8 N8 Ni3 161.5(7) . . ? C9 N9 Ni2 165.9(7) . . ? C13 N13 C24 116.4(8) . . ? C13 N13 Ni1 129.4(6) . . ? C24 N13 Ni1 114.2(6) . . ? C22 N14 C23 118.4(9) . . ? C22 N14 Ni1 128.8(8) . . ? C23 N14 Ni1 112.8(6) . . ? C29 N15 C40 115.7(8) . . ? C29 N15 Ni1 130.3(7) . . ? C40 N15 Ni1 114.0(6) . . ? C38 N16 C39 116.0(8) . . ? C38 N16 Ni1 128.6(7) . . ? C39 N16 Ni1 115.4(7) . . ? C54 N17 C55 117.2(8) . . ? C54 N17 Ni2 129.3(7) . . ? C55 N17 Ni2 113.4(6) . . ? C45 N18 C56 117.5(8) . . ? C45 N18 Ni2 128.4(6) . . ? C56 N18 Ni2 114.1(6) . . ? C61 N19 C72 119.6(9) . . ? C61 N19 Ni2 126.7(7) . . ? C72 N19 Ni2 113.6(6) . . ? C71 N20 C70 117.8(8) . . ? C71 N20 Ni2 114.8(6) . . ? C70 N20 Ni2 127.4(6) . . ? C93 N21 C104 117.1(7) . . ? C93 N21 Ni3 128.8(6) . . ? C104 N21 Ni3 113.4(5) . . ? C102 N22 C103 118.0(8) . . ? C102 N22 Ni3 128.4(7) . . ? C103 N22 Ni3 112.9(5) . . ? C77 N23 C88 115.9(8) . . ? C77 N23 Ni3 129.9(7) . . ? C88 N23 Ni3 114.2(6) . . ? C86 N24 C87 118.2(8) . . ? C86 N24 Ni3 127.5(7) . . ? C87 N24 Ni3 114.0(6) . . ? N1 C1 Mo1 173.2(8) . . ? N2 C2 Mo1 171.1(8) . . ? N3 C3 Mo1 176.7(9) . . ? N4 C4 Mo1 174.3(11) . . ? N5 C5 Mo1 174.7(9) . . ? N6 C6 Mo1 179.2(15) . . ? N7 C7 Mo2 178.6(9) . . ? N8 C8 Mo2 169.8(8) . . ? N9 C9 Mo2 172.4(8) . . ? N10 C10 Mo2 177.0(10) . . ? N11 C11 Mo2 175.9(9) . . ? N12 C12 Mo2 176.7(10) . . ? N13 C13 C14 125.2(9) . . ? C15 C14 C13 117.2(9) . . ? C15 C14 C25 124.1(9) . . ? C13 C14 C25 118.6(9) . . ? C16 C15 C14 118.3(9) . . ? C16 C15 C26 121.1(10) . . ? C14 C15 C26 120.5(10) . . ? C24 C16 C15 120.2(9) . . ? C24 C16 C17 116.7(10) . . ? C15 C16 C17 123.1(10) . . ? C18 C17 C16 123.3(11) . . ? C17 C18 C19 121.1(10) . . ? C23 C19 C20 118.6(10) . . ? C23 C19 C18 118.3(10) . . ? C20 C19 C18 123.1(10) . . ? C21 C20 C19 119.4(10) . . ? C21 C20 C27 119.6(11) . . ? C19 C20 C27 120.9(11) . . ? C20 C21 C22 118.0(10) . . ? C20 C21 C28 124.8(12) . . ? C22 C21 C28 117.2(12) . . ? N14 C22 C21 123.3(11) . . ? N14 C23 C19 122.3(9) . . ? N14 C23 C24 118.2(9) . . ? C19 C23 C24 119.5(9) . . ? N13 C24 C16 122.7(9) . . ? N13 C24 C23 116.2(9) . . ? C16 C24 C23 121.1(9) . . ? N15 C29 C30 126.0(9) . . ? C31 C30 C29 117.5(9) . . ? C31 C30 C41 123.5(9) . . ? C29 C30 C41 118.9(9) . . ? C30 C31 C32 118.8(10) . . ? C30 C31 C42 120.0(10) . . ? C32 C31 C42 121.2(10) . . ? C40 C32 C31 119.0(9) . . ? C40 C32 C33 117.1(10) . . ? C31 C32 C33 123.9(10) . . ? C34 C33 C32 122.3(10) . . ? C33 C34 C35 121.9(10) . . ? C39 C35 C34 117.0(10) . . ? C39 C35 C36 119.3(10) . . ? C34 C35 C36 123.5(9) . . ? C37 C36 C35 117.0(9) . . ? C37 C36 C44 122.5(10) . . ? C35 C36 C44 120.5(10) . . ? C36 C37 C38 119.8(10) . . ? C36 C37 C43 122.0(9) . . ? C38 C37 C43 118.2(9) . . ? N16 C38 C37 124.2(9) . . ? N16 C39 C35 123.4(10) . . ? N16 C39 C40 115.5(9) . . ? C35 C39 C40 121.1(10) . . ? N15 C40 C32 122.9(9) . . ? N15 C40 C39 116.6(9) . . ? C32 C40 C39 120.5(9) . . ? N18 C45 C46 124.6(9) . . ? C47 C46 C45 118.3(10) . . ? C47 C46 C57 123.0(9) . . ? C45 C46 C57 118.7(9) . . ? C46 C47 C48 118.2(9) . . ? C46 C47 C58 119.8(10) . . ? C48 C47 C58 122.0(9) . . ? C56 C48 C47 119.0(9) . . ? C56 C48 C49 116.4(10) . . ? C47 C48 C49 124.6(9) . . ? C50 C49 C48 122.9(10) . . ? C49 C50 C51 120.9(10) . . ? C52 C51 C55 119.4(9) . . ? C52 C51 C50 122.6(10) . . ? C55 C51 C50 117.9(9) . . ? C53 C52 C51 118.6(9) . . ? C53 C52 C60 121.6(10) . . ? C51 C52 C60 119.8(10) . . ? C52 C53 C54 118.1(9) . . ? C52 C53 C59 123.4(10) . . ? C54 C53 C59 118.5(10) . . ? N17 C54 C53 124.6(9) . . ? N17 C55 C51 122.0(9) . . ? N17 C55 C56 116.7(8) . . ? C51 C55 C56 121.3(9) . . ? N18 C56 C48 122.4(9) . . ? N18 C56 C55 117.0(8) . . ? C48 C56 C55 120.6(9) . . ? N19 C61 C62 121.5(10) . . ? C63 C62 C61 120.5(10) . . ? C63 C62 C73 122.5(11) . . ? C61 C62 C73 117.0(11) . . ? C62 C63 C64 117.6(10) . . ? C62 C63 C74 121.9(11) . . ? C64 C63 C74 120.5(12) . . ? C65 C64 C72 118.4(10) . . ? C65 C64 C63 124.0(11) . . ? C72 C64 C63 117.6(11) . . ? C66 C65 C64 122.8(10) . . ? C65 C66 C67 120.7(10) . . ? C71 C67 C66 118.2(9) . . ? C71 C67 C68 117.9(9) . . ? C66 C67 C68 123.9(10) . . ? C69 C68 C67 118.6(9) . . ? C69 C68 C75 118.5(10) . . ? C67 C68 C75 122.9(10) . . ? C70 C69 C68 118.2(9) . . ? C70 C69 C76 118.7(10) . . ? C68 C69 C76 123.1(9) . . ? N20 C70 C69 123.8(9) . . ? N20 C71 C67 123.8(9) . . ? N20 C71 C72 115.5(8) . . ? C67 C71 C72 120.7(9) . . ? N19 C72 C64 123.2(9) . . ? N19 C72 C71 117.7(9) . . ? C64 C72 C71 119.1(10) . . ? N23 C77 C78 126.3(10) . . ? C79 C78 C77 117.4(10) . . ? C79 C78 C89 124.1(10) . . ? C77 C78 C89 118.5(11) . . ? C78 C79 C80 119.2(9) . . ? C78 C79 C90 119.4(11) . . ? C80 C79 C90 121.3(11) . . ? C88 C80 C79 117.8(10) . . ? C88 C80 C81 118.1(10) . . ? C79 C80 C81 124.0(10) . . ? C82 C81 C80 120.8(10) . . ? C81 C82 C83 123.0(10) . . ? C87 C83 C84 118.3(9) . . ? C87 C83 C82 116.9(10) . . ? C84 C83 C82 124.7(10) . . ? C85 C84 C83 118.4(9) . . ? C85 C84 C91 119.7(11) . . ? C83 C84 C91 121.9(11) . . ? C84 C85 C86 119.0(10) . . ? C84 C85 C92 124.0(10) . . ? C86 C85 C92 116.7(11) . . ? N24 C86 C85 123.2(10) . . ? N24 C87 C83 122.8(9) . . ? N24 C87 C88 117.0(8) . . ? C83 C87 C88 120.2(9) . . ? N23 C88 C80 123.2(9) . . ? N23 C88 C87 115.9(8) . . ? C80 C88 C87 120.9(9) . . ? N21 C93 C94 124.2(8) . . ? C93 C94 C95 118.6(8) . . ? C93 C94 C105 119.2(8) . . ? C95 C94 C105 122.1(8) . . ? C96 C95 C94 117.9(9) . . ? C96 C95 C106 122.4(9) . . ? C94 C95 C106 119.7(8) . . ? C104 C96 C95 118.4(8) . . ? C104 C96 C97 117.7(8) . . ? C95 C96 C97 123.8(9) . . ? C98 C97 C96 121.7(10) . . ? C97 C98 C99 121.5(9) . . ? C103 C99 C98 118.4(8) . . ? C103 C99 C100 118.0(9) . . ? C98 C99 C100 123.6(9) . . ? C101 C100 C99 118.2(8) . . ? C101 C100 C108 121.5(9) . . ? C99 C100 C108 120.3(10) . . ? C100 C101 C102 119.6(9) . . ? C100 C101 C107 122.6(9) . . ? C102 C101 C107 117.8(9) . . ? N22 C102 C101 123.5(9) . . ? N22 C103 C99 122.7(8) . . ? N22 C103 C104 117.6(7) . . ? C99 C103 C104 119.6(9) . . ? N21 C104 C96 123.6(8) . . ? N21 C104 C103 115.4(8) . . ? C96 C104 C103 120.9(8) . . ? N25 C110 C109 166(4) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.910 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.168