# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1445 data_total _audit_creation_method SHELXL-97 _publ_contact_author_name 'Carlo Floriani' _publ_contact_author_address ; Institut de Chimie Min\'erale et Analytique BCH # 3307 Universit\'e de Lausanne CH-1015 Lausanne Switzerland ; _publ_contact_author_email 'carlo.floriani@icma.unil.ch' _publ_contact_author_fax '+4121 692 3905' _publ_contact_author_phone '+4121 692 3902' _publ_section_title ; Porphyrinogen tetraanion functioning as a polymetallic assembler: the nickel-meso-octaethylporphyrinogen binding four transition metal ions at the periphery ; loop_ _publ_author_name _publ_author_address 'Bonomo, Lucia' ; Institut de Chimie Min\'erale et Analytique BCH Universit\'e de Lausanne CH-1015 Lausanne Switzerland ; 'Solari, Euro' ; Institut de Chimie Min\'erale et Analytique BCH Universit\'e de Lausanne CH-1015 Lausanne Switzerland ; 'Martin, G\'eraldine' ; Institut de Chimie Min\'erale et Analytique BCH Universit\'e de Lausanne CH-1015 Lausanne Switzerland ; 'Scopelliti, Rosario' ; Institut de Chimie Min\'erale et Analytique BCH Universit\'e de Lausanne CH-1015 Lausanne Switzerland ; 'Floriani, Carlo' ; Institut de Chimie Min\'erale et Analytique BCH Universit\'e de Lausanne CH-1015 Lausanne Switzerland ; data_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H88 Li2 Mo2 N4 Ni O11, C4 H8 O' _chemical_formula_sum 'C66 H96 Li2 Mo2 N4 Ni O12' _chemical_formula_weight 1401.94 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' 'Li' 'Li' -0.0003 0.0001 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 50.392(4) _cell_length_b 11.6140(8) _cell_length_c 23.8148(12) _cell_angle_alpha 90.00 _cell_angle_beta 105.537(5) _cell_angle_gamma 90.00 _cell_volume 13428.3(15) _cell_formula_units_Z 8 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 5 _cell_measurement_theta_max 20 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.387 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5872 _exptl_absorpt_coefficient_mu 0.707 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 'KUMA diffractometer equipped with a CCD detector' _diffrn_measurement_method '2 runs (110 frames each) using omega scan, 1 run (300 frames) using phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38408 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0264 _diffrn_reflns_limit_h_min -57 _diffrn_reflns_limit_h_max 57 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.03 _reflns_number_total 11199 _reflns_number_gt 9809 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Kuma Diffraction Instruments GmbH, release 1.6.0, 1999' _computing_cell_refinement 'CrysAlis RED, Kuma Diffraction Instruments GmbH, release 1.6.0, 1999' _computing_data_reduction 'CrysAlis RED' _computing_structure_solution 'SIR97 (Altomare A. et al., J. Appl. Cryst., 1999, 32, 115-119)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker AXS, Inc., release 5.1, 1997' _computing_publication_material '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^)+(0.0542P)^2^+131.9335P] 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 SHELXL _refine_ls_extinction_coef 0.00016(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11199 _refine_ls_number_parameters 760 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0630 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1411 _refine_ls_wR_factor_gt 0.1303 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.007 _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 Ni1 Ni 0.110954(11) -0.11725(4) 0.26556(2) 0.01517(14) Uani 1 1 d . . . N1 N 0.08692(7) -0.0083(3) 0.28332(14) 0.0147(7) Uani 1 1 d . . . N2 N 0.09080(7) -0.1126(3) 0.18682(15) 0.0182(7) Uani 1 1 d . . . N3 N 0.13588(7) -0.2223(3) 0.24740(14) 0.0171(7) Uani 1 1 d . . . N4 N 0.12660(7) -0.1438(3) 0.34500(15) 0.0183(7) Uani 1 1 d . . . C1 C 0.09291(9) 0.0624(3) 0.33313(17) 0.0182(9) Uani 1 1 d . . . C2 C 0.06842(9) 0.1140(4) 0.33695(18) 0.0202(9) Uani 1 1 d . . . H2 H 0.0665 0.1659 0.3664 0.024 Uiso 1 1 calc R . . C3 C 0.04676(9) 0.0748(4) 0.28861(18) 0.0202(9) Uani 1 1 d . . . H3 H 0.0279 0.0958 0.2800 0.024 Uiso 1 1 calc R . . C4 C 0.05878(8) -0.0009(3) 0.25640(17) 0.0158(8) Uani 1 1 d . . . C5 C 0.04520(8) -0.0865(3) 0.20948(18) 0.0178(9) Uani 1 1 d . . . C6 C 0.06250(9) -0.1054(3) 0.16722(18) 0.0186(9) Uani 1 1 d . . . C7 C 0.05455(9) -0.1235(4) 0.10789(18) 0.0218(9) Uani 1 1 d . . . H7 H 0.0362 -0.1234 0.0835 0.026 Uiso 1 1 calc R . . C8 C 0.07889(9) -0.1423(4) 0.09018(18) 0.0230(9) Uani 1 1 d . . . H8 H 0.0800 -0.1572 0.0517 0.028 Uiso 1 1 calc R . . C9 C 0.10054(9) -0.1348(4) 0.13943(18) 0.0194(9) Uani 1 1 d . . . C10 C 0.13159(9) -0.1369(4) 0.14794(18) 0.0211(9) Uani 1 1 d . . . C11 C 0.14257(9) -0.2280(4) 0.19435(18) 0.0179(9) Uani 1 1 d . . . C12 C 0.15543(10) -0.3342(4) 0.1913(2) 0.0263(10) Uani 1 1 d . . . H12 H 0.1622 -0.3607 0.1599 0.032 Uiso 1 1 calc R . . C13 C 0.15649(9) -0.3946(4) 0.24380(19) 0.0234(9) Uani 1 1 d . . . H13 H 0.1641 -0.4691 0.2540 0.028 Uiso 1 1 calc R . . C14 C 0.14436(9) -0.3245(3) 0.27751(18) 0.0195(9) Uani 1 1 d . . . C15 C 0.13493(9) -0.3550(4) 0.33144(18) 0.0208(9) Uani 1 1 d . . . C16 C 0.13529(9) -0.2494(4) 0.36957(18) 0.0208(9) Uani 1 1 d . . . C17 C 0.14083(10) -0.2420(4) 0.42922(19) 0.0259(10) Uani 1 1 d . . . H17 H 0.1470 -0.3027 0.4563 0.031 Uiso 1 1 calc R . . C18 C 0.13561(10) -0.1271(4) 0.44278(19) 0.0257(10) Uani 1 1 d . . . H18 H 0.1377 -0.0958 0.4806 0.031 Uiso 1 1 calc R . . C19 C 0.12694(9) -0.0692(4) 0.39039(17) 0.0195(9) Uani 1 1 d . . . C20 C 0.12112(9) 0.0573(4) 0.37667(17) 0.0208(9) Uani 1 1 d . . . C21 C 0.04302(9) -0.2005(3) 0.24306(19) 0.0209(9) Uani 1 1 d . . . H21A H 0.0617 -0.2211 0.2670 0.025 Uiso 1 1 calc R . . H21B H 0.0316 -0.1851 0.2701 0.025 Uiso 1 1 calc R . . C22 C 0.03108(12) -0.3037(4) 0.2061(2) 0.0390(13) Uani 1 1 d . . . H22A H 0.0114 -0.2915 0.1886 0.058 Uiso 1 1 calc R . . H22B H 0.0338 -0.3728 0.2305 0.058 Uiso 1 1 calc R . . H22C H 0.0404 -0.3135 0.1752 0.058 Uiso 1 1 calc R . . C23 C 0.01530(9) -0.0513(4) 0.17680(18) 0.0211(9) Uani 1 1 d . . . H23A H 0.0076 -0.1127 0.1483 0.025 Uiso 1 1 calc R . . H23B H 0.0043 -0.0504 0.2056 0.025 Uiso 1 1 calc R . . C24 C 0.01075(9) 0.0635(4) 0.14440(19) 0.0244(10) Uani 1 1 d . . . H24A H 0.0163 0.1267 0.1724 0.037 Uiso 1 1 calc R . . H24B H -0.0088 0.0718 0.1238 0.037 Uiso 1 1 calc R . . H24C H 0.0218 0.0658 0.1162 0.037 Uiso 1 1 calc R . . C25 C 0.13767(10) -0.1716(4) 0.08993(19) 0.0283(10) Uani 1 1 d . . . H25A H 0.1318 -0.2525 0.0813 0.034 Uiso 1 1 calc R . . H25B H 0.1262 -0.1232 0.0584 0.034 Uiso 1 1 calc R . . C26 C 0.16778(11) -0.1606(5) 0.0884(2) 0.0392(13) Uani 1 1 d . . . H26A H 0.1729 -0.0790 0.0898 0.059 Uiso 1 1 calc R . . H26B H 0.1700 -0.1951 0.0525 0.059 Uiso 1 1 calc R . . H26C H 0.1797 -0.2006 0.1221 0.059 Uiso 1 1 calc R . . C27 C 0.14321(9) -0.0153(4) 0.16783(19) 0.0244(10) Uani 1 1 d . . . H27A H 0.1402 0.0013 0.2064 0.029 Uiso 1 1 calc R . . H27B H 0.1633 -0.0157 0.1725 0.029 Uiso 1 1 calc R . . C28 C 0.13022(11) 0.0812(4) 0.1257(2) 0.0328(11) Uani 1 1 d . . . H28A H 0.1350 0.0708 0.0888 0.049 Uiso 1 1 calc R . . H28B H 0.1372 0.1557 0.1427 0.049 Uiso 1 1 calc R . . H28C H 0.1102 0.0788 0.1186 0.049 Uiso 1 1 calc R . . C29 C 0.10450(9) -0.3985(4) 0.30664(19) 0.0236(9) Uani 1 1 d . . . H29A H 0.0942 -0.3402 0.2789 0.028 Uiso 1 1 calc R . . H29B H 0.1049 -0.4702 0.2844 0.028 Uiso 1 1 calc R . . C30 C 0.08898(11) -0.4217(5) 0.3515(2) 0.0354(12) Uani 1 1 d . . . H30A H 0.0973 -0.4875 0.3756 0.053 Uiso 1 1 calc R . . H30B H 0.0697 -0.4391 0.3318 0.053 Uiso 1 1 calc R . . H30C H 0.0898 -0.3536 0.3762 0.053 Uiso 1 1 calc R . . C31 C 0.15178(10) -0.4554(4) 0.3661(2) 0.0274(10) Uani 1 1 d . . . H31A H 0.1437 -0.4747 0.3985 0.033 Uiso 1 1 calc R . . H31B H 0.1492 -0.5233 0.3401 0.033 Uiso 1 1 calc R . . C32 C 0.18271(11) -0.4378(5) 0.3919(2) 0.0375(12) Uani 1 1 d . . . H32A H 0.1918 -0.4330 0.3603 0.056 Uiso 1 1 calc R . . H32B H 0.1903 -0.5029 0.4173 0.056 Uiso 1 1 calc R . . H32C H 0.1859 -0.3663 0.4146 0.056 Uiso 1 1 calc R . . C33 C 0.14421(10) 0.1066(4) 0.3520(2) 0.0269(10) Uani 1 1 d . . . H33A H 0.1438 0.0670 0.3150 0.032 Uiso 1 1 calc R . . H33B H 0.1407 0.1894 0.3434 0.032 Uiso 1 1 calc R . . C34 C 0.17286(11) 0.0925(5) 0.3942(3) 0.0436(14) Uani 1 1 d . . . H34A H 0.1739 0.1365 0.4298 0.065 Uiso 1 1 calc R . . H34B H 0.1868 0.1210 0.3757 0.065 Uiso 1 1 calc R . . H34C H 0.1762 0.0109 0.4039 0.065 Uiso 1 1 calc R . . C35 C 0.12039(10) 0.1226(4) 0.43269(19) 0.0271(10) Uani 1 1 d . . . H35A H 0.1040 0.0968 0.4446 0.032 Uiso 1 1 calc R . . H35B H 0.1368 0.1002 0.4640 0.032 Uiso 1 1 calc R . . C36 C 0.11964(12) 0.2543(4) 0.4284(2) 0.0353(12) Uani 1 1 d . . . H36A H 0.1374 0.2825 0.4247 0.053 Uiso 1 1 calc R . . H36B H 0.1160 0.2867 0.4636 0.053 Uiso 1 1 calc R . . H36C H 0.1050 0.2778 0.3942 0.053 Uiso 1 1 calc R . . Mo1 Mo 0.077129(8) 0.18617(3) 0.248528(15) 0.01828(12) Uani 1 1 d . . . C37 C 0.06842(9) 0.2053(4) 0.1665(2) 0.0245(10) Uani 1 1 d . . . O1 O 0.06279(8) 0.2212(3) 0.11542(14) 0.0337(8) Uani 1 1 d . . . C38 C 0.10958(10) 0.2750(4) 0.2468(2) 0.0285(11) Uani 1 1 d . . . O2 O 0.12838(8) 0.3307(3) 0.24339(18) 0.0458(10) Uani 1 1 d . . . C39 C 0.05807(11) 0.3290(4) 0.2478(2) 0.0301(11) Uani 1 1 d . . . O3 O 0.04559(9) 0.4142(3) 0.24779(19) 0.0500(11) Uani 1 1 d . . . Mo2 Mo 0.185514(8) -0.22780(3) 0.268877(17) 0.02333(13) Uani 1 1 d . . . C40 C 0.20409(11) -0.1012(5) 0.2474(2) 0.0397(13) Uani 1 1 d . . . O4 O 0.21699(9) -0.0271(4) 0.2324(2) 0.0664(15) Uani 1 1 d . . . C41 C 0.21911(11) -0.3000(5) 0.2729(3) 0.0425(14) Uani 1 1 d . . . O5 O 0.24050(9) -0.3455(5) 0.2744(3) 0.0765(16) Uani 1 1 d . . . C42 C 0.20317(12) -0.1786(5) 0.3486(2) 0.0441(14) Uani 1 1 d . . . O6 O 0.21502(11) -0.1491(5) 0.39452(19) 0.0765(16) Uani 1 1 d . . . Li1 Li 0.22207(19) 0.1108(8) 0.1932(4) 0.041(2) Uani 1 1 d . . . O7 O 0.20058(11) 0.2259(5) 0.2161(3) 0.0732(15) Uani 1 1 d . . . C43 C 0.1910(2) 0.2068(9) 0.2678(4) 0.095(3) Uani 1 1 d . . . H43A H 0.1994 0.1362 0.2884 0.114 Uiso 1 1 calc R . . H43B H 0.1707 0.1980 0.2570 0.114 Uiso 1 1 calc R . . C44 C 0.19929(17) 0.3074(6) 0.3050(4) 0.069(2) Uani 1 1 d . . . H44A H 0.1829 0.3527 0.3067 0.082 Uiso 1 1 calc R . . H44B H 0.2090 0.2830 0.3451 0.082 Uiso 1 1 calc R . . C45 C 0.2174(2) 0.3765(7) 0.2804(5) 0.085(3) Uani 1 1 d . . . H45A H 0.2370 0.3555 0.2970 0.102 Uiso 1 1 calc R . . H45B H 0.2149 0.4598 0.2862 0.102 Uiso 1 1 calc R . . C46 C 0.2070(3) 0.3423(9) 0.2153(5) 0.113(4) Uani 1 1 d . . . H46A H 0.1906 0.3877 0.1954 0.136 Uiso 1 1 calc R . . H46B H 0.2216 0.3548 0.1950 0.136 Uiso 1 1 calc R . . O8 O 0.21569(11) 0.0960(5) 0.1120(2) 0.0682(14) Uani 1 1 d . . . C47 C 0.1997(2) 0.1751(11) 0.0704(4) 0.102(4) Uani 1 1 d . . . H47A H 0.1964 0.2472 0.0897 0.122 Uiso 1 1 calc R . . H47B H 0.1817 0.1409 0.0498 0.122 Uiso 1 1 calc R . . C48 C 0.2161(2) 0.1968(11) 0.0309(4) 0.108(4) Uani 1 1 d . . . H48A H 0.2273 0.2672 0.0424 0.130 Uiso 1 1 calc R . . H48B H 0.2042 0.2070 -0.0093 0.130 Uiso 1 1 calc R . . C49 C 0.2342(3) 0.0940(13) 0.0341(5) 0.145(6) Uani 1 1 d . . . H49A H 0.2269 0.0429 0.0002 0.174 Uiso 1 1 calc R . . H49B H 0.2531 0.1180 0.0343 0.174 Uiso 1 1 calc R . . C50 C 0.2345(3) 0.0360(10) 0.0866(4) 0.105(4) Uani 1 1 d . . . H50A H 0.2532 0.0366 0.1134 0.126 Uiso 1 1 calc R . . H50B H 0.2286 -0.0450 0.0784 0.126 Uiso 1 1 calc R . . Li2 Li 0.0441(2) 0.3199(8) 0.0520(4) 0.038(2) Uani 1 1 d . . . O9 O 0.03875(8) 0.2272(3) -0.01615(15) 0.0361(8) Uani 1 1 d . . . C51 C 0.04724(14) 0.2539(5) -0.0679(2) 0.0434(14) Uani 1 1 d . . . H51A H 0.0616 0.3146 -0.0594 0.052 Uiso 1 1 calc R . . H51B H 0.0313 0.2819 -0.0991 0.052 Uiso 1 1 calc R . . C52 C 0.05862(12) 0.1442(5) -0.0870(2) 0.0377(12) Uani 1 1 d . . . H52A H 0.0771 0.1575 -0.0930 0.045 Uiso 1 1 calc R . . H52B H 0.0462 0.1144 -0.1237 0.045 Uiso 1 1 calc R . . C53 C 0.06018(12) 0.0615(5) -0.0368(2) 0.0389(13) Uani 1 1 d . . . H53A H 0.0567 -0.0187 -0.0509 0.047 Uiso 1 1 calc R . . H53B H 0.0784 0.0654 -0.0079 0.047 Uiso 1 1 calc R . . C54 C 0.03779(13) 0.1038(5) -0.0113(2) 0.0388(13) Uani 1 1 d . . . H54A H 0.0196 0.0736 -0.0334 0.047 Uiso 1 1 calc R . . H54B H 0.0413 0.0800 0.0300 0.047 Uiso 1 1 calc R . . O10 O 0.00901(9) 0.3691(4) 0.06060(18) 0.0590(13) Uani 1 1 d . . . C55 C -0.01599(17) 0.3138(10) 0.0295(3) 0.091(3) Uani 1 1 d . . . H55A H -0.0132 0.2295 0.0290 0.109 Uiso 1 1 calc R . . H55B H -0.0216 0.3417 -0.0112 0.109 Uiso 1 1 calc R . . C56 C -0.03736(18) 0.3401(10) 0.0584(4) 0.087(3) Uani 1 1 d . . . H56A H -0.0481 0.2703 0.0617 0.104 Uiso 1 1 calc R . . H56B H -0.0501 0.3996 0.0365 0.104 Uiso 1 1 calc R . . C57 C -0.0224(3) 0.3829(10) 0.1165(4) 0.110(4) Uani 1 1 d . . . H57A H -0.0185 0.3195 0.1453 0.132 Uiso 1 1 calc R . . H57B H -0.0332 0.4430 0.1300 0.132 Uiso 1 1 calc R . . C58 C 0.0038(2) 0.4318(11) 0.1082(4) 0.111(4) Uani 1 1 d . . . H58A H 0.0016 0.5150 0.0989 0.133 Uiso 1 1 calc R . . H58B H 0.0191 0.4216 0.1439 0.133 Uiso 1 1 calc R . . O11 O 0.07056(13) 0.4408(4) 0.0540(2) 0.0664(14) Uani 1 1 d . . . C59 C 0.07174(19) 0.5425(6) 0.0880(3) 0.077(3) Uani 1 1 d . . . H59A H 0.0774 0.6079 0.0671 0.080 Uiso 1 1 calc R . . H59B H 0.0531 0.5595 0.0920 0.080 Uiso 1 1 calc R . . C60 C 0.0897(2) 0.5340(8) 0.1424(4) 0.102(3) Uani 1 1 d DU . . H60A H 0.0828 0.4863 0.1700 0.080 Uiso 1 1 calc R . . H60B H 0.0968 0.6090 0.1600 0.080 Uiso 1 1 calc R . . C61 C 0.1112(3) 0.4645(15) 0.1110(6) 0.177(6) Uani 1 1 d DU . . H61A H 0.1241 0.5214 0.1018 0.080 Uiso 1 1 calc R . . H61B H 0.1223 0.4095 0.1396 0.080 Uiso 1 1 calc R . . C62 C 0.0983(2) 0.4024(10) 0.0586(5) 0.107(4) Uani 1 1 d DU . . H62A H 0.1003 0.3180 0.0638 0.080 Uiso 1 1 calc R . . H62B H 0.1050 0.4272 0.0251 0.080 Uiso 1 1 calc R . . O12 O 0.1803(6) -0.520(3) 0.5396(12) 0.438(15) Uiso 1 1 d D . . C63 C 0.2051(3) -0.5455(17) 0.6004(7) 0.192(7) Uiso 1 1 d D . . H63A H 0.2070 -0.4696 0.6200 0.080 Uiso 1 1 calc R . . H63B H 0.1953 -0.5939 0.6227 0.080 Uiso 1 1 calc R . . C64 C 0.2355(5) -0.594(2) 0.6221(10) 0.325(16) Uiso 1 1 d D . . H64A H 0.2378 -0.6460 0.6560 0.080 Uiso 1 1 calc R . . H64B H 0.2493 -0.5315 0.6317 0.080 Uiso 1 1 calc R . . C65 C 0.2368(5) -0.666(2) 0.5616(10) 0.313(15) Uiso 1 1 d D . . H65A H 0.2519 -0.6421 0.5447 0.080 Uiso 1 1 calc R . . H65B H 0.2353 -0.7504 0.5639 0.080 Uiso 1 1 calc R . . C66 C 0.2095(4) -0.6025(19) 0.5368(8) 0.228(9) Uiso 1 1 d D . . H66A H 0.1995 -0.6668 0.5131 0.080 Uiso 1 1 calc R . . H66B H 0.2155 -0.5544 0.5081 0.080 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 Ni1 0.0166(3) 0.0160(3) 0.0128(3) -0.00009(19) 0.0038(2) 0.00172(19) N1 0.0186(18) 0.0109(16) 0.0143(16) 0.0009(12) 0.0038(14) -0.0009(13) N2 0.0179(18) 0.0184(17) 0.0186(17) 0.0007(14) 0.0051(14) 0.0021(14) N3 0.0148(18) 0.0215(18) 0.0139(16) 0.0011(14) 0.0016(14) 0.0005(14) N4 0.0220(19) 0.0164(17) 0.0162(17) -0.0008(14) 0.0045(14) 0.0022(14) C1 0.025(2) 0.016(2) 0.0124(18) 0.0023(15) 0.0035(17) -0.0003(16) C2 0.026(2) 0.016(2) 0.020(2) -0.0014(16) 0.0083(18) -0.0007(17) C3 0.021(2) 0.017(2) 0.025(2) 0.0005(17) 0.0098(18) -0.0019(16) C4 0.016(2) 0.0150(19) 0.0181(19) 0.0007(16) 0.0069(16) -0.0003(15) C5 0.011(2) 0.018(2) 0.023(2) -0.0050(17) 0.0025(16) -0.0025(15) C6 0.019(2) 0.0143(19) 0.022(2) 0.0002(16) 0.0040(17) -0.0001(16) C7 0.019(2) 0.023(2) 0.020(2) -0.0030(17) -0.0014(17) 0.0033(17) C8 0.029(2) 0.025(2) 0.0136(19) -0.0032(17) 0.0021(18) 0.0046(18) C9 0.024(2) 0.019(2) 0.018(2) 0.0026(16) 0.0109(17) 0.0039(17) C10 0.022(2) 0.026(2) 0.017(2) 0.0017(17) 0.0082(17) 0.0021(17) C11 0.016(2) 0.022(2) 0.018(2) -0.0029(16) 0.0082(17) 0.0014(16) C12 0.029(3) 0.028(2) 0.022(2) -0.0046(18) 0.0069(19) 0.0041(19) C13 0.024(2) 0.022(2) 0.025(2) 0.0013(17) 0.0082(19) 0.0033(17) C14 0.019(2) 0.017(2) 0.021(2) 0.0011(16) 0.0031(17) 0.0029(16) C15 0.025(2) 0.017(2) 0.021(2) 0.0043(17) 0.0062(18) 0.0039(17) C16 0.025(2) 0.019(2) 0.019(2) 0.0024(17) 0.0059(18) 0.0017(17) C17 0.032(3) 0.027(2) 0.018(2) 0.0059(18) 0.0067(19) 0.0050(19) C18 0.030(3) 0.030(2) 0.015(2) 0.0007(18) 0.0019(18) 0.0031(19) C19 0.020(2) 0.022(2) 0.016(2) 0.0000(16) 0.0036(17) -0.0016(17) C20 0.026(2) 0.020(2) 0.0143(19) -0.0018(16) 0.0029(17) -0.0004(17) C21 0.022(2) 0.014(2) 0.025(2) 0.0038(17) 0.0037(18) -0.0018(16) C22 0.056(4) 0.019(2) 0.035(3) 0.000(2) 0.000(3) -0.005(2) C23 0.019(2) 0.020(2) 0.020(2) -0.0048(17) -0.0007(17) -0.0012(17) C24 0.024(2) 0.024(2) 0.024(2) 0.0033(18) 0.0031(18) 0.0053(18) C25 0.034(3) 0.035(3) 0.018(2) 0.0028(19) 0.010(2) 0.004(2) C26 0.037(3) 0.057(3) 0.031(3) 0.005(2) 0.021(2) 0.008(3) C27 0.023(2) 0.026(2) 0.025(2) 0.0025(18) 0.0077(19) -0.0016(18) C28 0.039(3) 0.031(3) 0.028(2) 0.004(2) 0.009(2) 0.000(2) C29 0.024(2) 0.019(2) 0.028(2) 0.0024(17) 0.0066(19) -0.0004(17) C30 0.036(3) 0.037(3) 0.038(3) -0.002(2) 0.019(2) -0.004(2) C31 0.035(3) 0.022(2) 0.026(2) 0.0072(18) 0.009(2) 0.0086(19) C32 0.033(3) 0.039(3) 0.034(3) 0.008(2) -0.001(2) 0.016(2) C33 0.027(3) 0.026(2) 0.026(2) 0.0007(18) 0.004(2) -0.0057(19) C34 0.025(3) 0.057(4) 0.043(3) 0.004(3) -0.001(2) -0.006(2) C35 0.036(3) 0.024(2) 0.019(2) -0.0066(18) 0.0028(19) -0.0008(19) C36 0.050(3) 0.023(2) 0.029(3) -0.008(2) 0.003(2) -0.003(2) Mo1 0.0227(2) 0.01343(19) 0.0183(2) 0.00048(13) 0.00486(15) -0.00077(13) C37 0.025(2) 0.018(2) 0.032(3) -0.0020(18) 0.008(2) -0.0007(17) O1 0.042(2) 0.038(2) 0.0185(17) 0.0037(14) 0.0041(15) -0.0035(16) C38 0.035(3) 0.022(2) 0.025(2) 0.0034(18) 0.001(2) 0.002(2) O2 0.034(2) 0.039(2) 0.061(3) 0.0142(19) 0.0062(19) -0.0144(17) C39 0.035(3) 0.024(2) 0.030(2) 0.0009(19) 0.005(2) -0.005(2) O3 0.063(3) 0.0211(19) 0.064(3) 0.0020(18) 0.013(2) 0.0171(18) Mo2 0.0179(2) 0.0284(2) 0.0237(2) 0.00238(15) 0.00556(16) 0.00338(15) C40 0.029(3) 0.049(3) 0.034(3) 0.010(2) -0.004(2) 0.001(2) O4 0.042(2) 0.069(3) 0.078(3) 0.035(3) 0.000(2) -0.022(2) C41 0.025(3) 0.040(3) 0.062(4) 0.007(3) 0.010(3) 0.003(2) O5 0.031(2) 0.066(3) 0.134(5) 0.003(3) 0.024(3) 0.018(2) C42 0.037(3) 0.056(4) 0.037(3) 0.003(3) 0.007(3) -0.003(3) O6 0.072(3) 0.107(4) 0.034(2) -0.014(3) -0.014(2) -0.016(3) Li1 0.032(5) 0.039(5) 0.055(6) 0.005(4) 0.014(4) -0.002(4) O7 0.067(3) 0.070(3) 0.082(4) -0.014(3) 0.018(3) 0.012(3) C43 0.101(7) 0.097(7) 0.116(8) -0.051(6) 0.080(6) -0.035(5) C44 0.068(5) 0.046(4) 0.092(6) -0.009(4) 0.022(4) -0.007(3) C45 0.087(6) 0.046(4) 0.131(8) -0.013(5) 0.047(6) -0.010(4) C46 0.154(11) 0.075(7) 0.121(9) 0.043(6) 0.058(8) 0.038(7) O8 0.084(4) 0.077(3) 0.051(3) 0.007(2) 0.029(3) 0.001(3) C47 0.075(6) 0.166(11) 0.060(5) 0.029(6) 0.009(5) 0.013(6) C48 0.107(8) 0.146(10) 0.077(6) 0.048(6) 0.033(6) 0.021(7) C49 0.167(12) 0.205(15) 0.079(7) 0.064(8) 0.060(8) 0.100(11) C50 0.149(10) 0.114(8) 0.067(5) 0.000(5) 0.056(6) 0.038(7) Li2 0.054(6) 0.037(5) 0.025(4) 0.000(4) 0.012(4) 0.012(4) O9 0.058(2) 0.0294(18) 0.0254(17) -0.0008(14) 0.0195(17) 0.0041(16) C51 0.067(4) 0.040(3) 0.027(3) 0.003(2) 0.019(3) 0.003(3) C52 0.042(3) 0.044(3) 0.032(3) -0.002(2) 0.017(2) 0.007(2) C53 0.046(3) 0.035(3) 0.034(3) -0.001(2) 0.009(2) 0.007(2) C54 0.056(4) 0.034(3) 0.030(3) -0.004(2) 0.017(2) -0.003(2) O10 0.055(3) 0.075(3) 0.043(2) -0.017(2) 0.007(2) 0.032(2) C55 0.064(5) 0.149(9) 0.051(4) -0.023(5) 0.001(4) 0.011(5) C56 0.065(5) 0.140(9) 0.066(5) 0.021(5) 0.036(4) 0.009(5) C57 0.140(10) 0.123(9) 0.081(7) 0.009(6) 0.053(7) 0.059(8) C58 0.081(7) 0.158(10) 0.096(7) -0.072(7) 0.030(6) 0.027(7) O11 0.119(5) 0.031(2) 0.055(3) -0.0049(19) 0.034(3) -0.016(2) C59 0.101(6) 0.044(4) 0.065(5) -0.019(3) -0.012(4) 0.013(4) C60 0.122(8) 0.085(6) 0.068(5) 0.015(4) -0.028(5) -0.047(5) C61 0.119(10) 0.192(14) 0.181(13) -0.037(10) -0.025(8) -0.029(9) C62 0.110(8) 0.097(7) 0.140(9) -0.032(6) 0.077(7) -0.050(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N4 1.870(3) . ? Ni1 N1 1.877(3) . ? Ni1 N2 1.879(3) . ? Ni1 N3 1.883(4) . ? N1 C4 1.394(5) . ? N1 C1 1.407(5) . ? N1 Mo1 2.410(3) . ? N2 C9 1.370(5) . ? N2 C6 1.379(5) . ? N3 C14 1.394(5) . ? N3 C11 1.394(5) . ? N3 Mo2 2.416(3) . ? N4 C16 1.379(5) . ? N4 C19 1.382(5) . ? C1 C2 1.397(6) . ? C1 C20 1.520(6) . ? C1 Mo1 2.429(4) . ? C2 C3 1.432(6) . ? C2 Mo1 2.413(4) . ? C3 C4 1.406(6) . ? C3 Mo1 2.390(4) . ? C4 C5 1.515(5) . ? C4 Mo1 2.388(4) . ? C5 C6 1.514(6) . ? C5 C23 1.554(5) . ? C5 C21 1.566(6) . ? C6 C7 1.377(6) . ? C7 C8 1.417(7) . ? C8 C9 1.374(6) . ? C9 C10 1.523(6) . ? C10 C11 1.523(6) . ? C10 C25 1.546(6) . ? C10 C27 1.553(6) . ? C11 C12 1.404(6) . ? C11 Mo2 2.403(4) . ? C12 C13 1.423(7) . ? C12 Mo2 2.396(4) . ? C13 C14 1.394(6) . ? C13 Mo2 2.405(5) . ? C14 C15 1.526(6) . ? C14 Mo2 2.415(4) . ? C15 C16 1.523(6) . ? C15 C31 1.545(6) . ? C15 C29 1.572(6) . ? C16 C17 1.375(6) . ? C17 C18 1.414(7) . ? C18 C19 1.381(6) . ? C19 C20 1.517(6) . ? C20 C35 1.544(6) . ? C20 C33 1.546(7) . ? C21 C22 1.513(6) . ? C23 C24 1.527(6) . ? C25 C26 1.533(7) . ? C27 C28 1.530(6) . ? C29 C30 1.508(7) . ? C31 C32 1.528(7) . ? C33 C34 1.530(6) . ? C35 C36 1.532(7) . ? Mo1 C37 1.896(5) . ? Mo1 C39 1.914(5) . ? Mo1 C38 1.943(5) . ? C37 O1 1.188(6) . ? O1 Li2 1.930(9) . ? C38 O2 1.168(6) . ? C39 O3 1.172(6) . ? Mo2 C41 1.869(6) . ? Mo2 C40 1.886(6) . ? Mo2 C42 1.954(6) . ? C40 O4 1.190(7) . ? O4 Li1 1.906(10) . ? C41 O5 1.192(7) . ? O5 Li1 1.905(10) 4_545 ? C42 O6 1.149(7) . ? Li1 O8 1.881(11) . ? Li1 O7 1.891(11) . ? Li1 O5 1.905(10) 4 ? O7 C46 1.392(12) . ? O7 C43 1.455(10) . ? C43 C44 1.457(11) . ? C44 C45 1.452(11) . ? C45 C46 1.549(14) . ? O8 C47 1.431(10) . ? O8 C50 1.434(10) . ? C47 C48 1.432(13) . ? C48 C49 1.493(15) . ? C49 C50 1.416(13) . ? Li2 O9 1.905(9) . ? Li2 O10 1.920(11) . ? Li2 O11 1.929(11) . ? O9 C54 1.440(6) . ? O9 C51 1.443(6) . ? C51 C52 1.516(8) . ? C52 C53 1.520(7) . ? C53 C54 1.500(8) . ? O10 C58 1.430(8) . ? O10 C55 1.431(10) . ? C55 C56 1.457(11) . ? C56 C57 1.473(13) . ? C57 C58 1.498(15) . ? O11 C59 1.425(8) . ? O11 C62 1.441(12) . ? C59 C60 1.372(10) . ? C60 C61 1.680(14) . ? C61 C62 1.436(12) . ? O12 C63 1.67(3) . ? O12 C66 1.78(3) . ? C63 C64 1.58(2) . ? C64 C65 1.68(3) . ? C65 C66 1.53(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 N4 Ni1 N1 90.33(15) . . ? N4 Ni1 N2 169.48(16) . . ? N1 Ni1 N2 89.80(14) . . ? N4 Ni1 N3 89.95(15) . . ? N1 Ni1 N3 177.98(15) . . ? N2 Ni1 N3 90.28(15) . . ? C4 N1 C1 108.3(3) . . ? C4 N1 Ni1 125.2(3) . . ? C1 N1 Ni1 125.3(3) . . ? C4 N1 Mo1 72.2(2) . . ? C1 N1 Mo1 73.8(2) . . ? Ni1 N1 Mo1 129.75(17) . . ? C9 N2 C6 107.4(3) . . ? C9 N2 Ni1 126.8(3) . . ? C6 N2 Ni1 125.0(3) . . ? C14 N3 C11 108.1(3) . . ? C14 N3 Ni1 124.4(3) . . ? C11 N3 Ni1 125.2(3) . . ? C14 N3 Mo2 73.2(2) . . ? C11 N3 Mo2 72.7(2) . . ? Ni1 N3 Mo2 133.24(17) . . ? C16 N4 C19 106.9(3) . . ? C16 N4 Ni1 125.1(3) . . ? C19 N4 Ni1 127.0(3) . . ? C2 C1 N1 108.1(4) . . ? C2 C1 C20 130.8(4) . . ? N1 C1 C20 120.2(4) . . ? C2 C1 Mo1 72.6(2) . . ? N1 C1 Mo1 72.4(2) . . ? C20 C1 Mo1 128.8(3) . . ? C1 C2 C3 107.9(4) . . ? C1 C2 Mo1 73.9(2) . . ? C3 C2 Mo1 71.7(2) . . ? C4 C3 C2 106.9(4) . . ? C4 C3 Mo1 72.8(2) . . ? C2 C3 Mo1 73.6(2) . . ? N1 C4 C3 108.8(3) . . ? N1 C4 C5 120.1(3) . . ? C3 C4 C5 129.6(4) . . ? N1 C4 Mo1 74.0(2) . . ? C3 C4 Mo1 73.0(2) . . ? C5 C4 Mo1 130.3(3) . . ? C6 C5 C4 111.0(3) . . ? C6 C5 C23 111.0(3) . . ? C4 C5 C23 112.5(3) . . ? C6 C5 C21 110.4(3) . . ? C4 C5 C21 104.9(3) . . ? C23 C5 C21 106.7(3) . . ? C7 C6 N2 109.2(4) . . ? C7 C6 C5 130.0(4) . . ? N2 C6 C5 120.7(4) . . ? C6 C7 C8 107.0(4) . . ? C9 C8 C7 106.8(4) . . ? N2 C9 C8 109.7(4) . . ? N2 C9 C10 118.4(4) . . ? C8 C9 C10 131.7(4) . . ? C11 C10 C9 105.6(3) . . ? C11 C10 C25 110.3(4) . . ? C9 C10 C25 109.1(3) . . ? C11 C10 C27 112.1(3) . . ? C9 C10 C27 108.4(4) . . ? C25 C10 C27 111.1(4) . . ? N3 C11 C12 108.4(4) . . ? N3 C11 C10 119.7(4) . . ? C12 C11 C10 130.9(4) . . ? N3 C11 Mo2 73.7(2) . . ? C12 C11 Mo2 72.7(2) . . ? C10 C11 Mo2 128.0(3) . . ? C11 C12 C13 107.2(4) . . ? C11 C12 Mo2 73.3(2) . . ? C13 C12 Mo2 73.1(3) . . ? C14 C13 C12 107.4(4) . . ? C14 C13 Mo2 73.6(3) . . ? C12 C13 Mo2 72.4(3) . . ? N3 C14 C13 108.8(4) . . ? N3 C14 C15 120.6(4) . . ? C13 C14 C15 129.3(4) . . ? N3 C14 Mo2 73.2(2) . . ? C13 C14 Mo2 72.8(3) . . ? C15 C14 Mo2 130.4(3) . . ? C16 C15 C14 111.0(3) . . ? C16 C15 C31 111.8(3) . . ? C14 C15 C31 112.0(4) . . ? C16 C15 C29 109.7(4) . . ? C14 C15 C29 104.5(3) . . ? C31 C15 C29 107.4(4) . . ? C17 C16 N4 109.6(4) . . ? C17 C16 C15 129.3(4) . . ? N4 C16 C15 120.8(4) . . ? C16 C17 C18 107.3(4) . . ? C19 C18 C17 106.6(4) . . ? C18 C19 N4 109.6(4) . . ? C18 C19 C20 131.5(4) . . ? N4 C19 C20 118.5(4) . . ? C19 C20 C1 106.0(3) . . ? C19 C20 C35 109.7(3) . . ? C1 C20 C35 109.6(4) . . ? C19 C20 C33 108.6(4) . . ? C1 C20 C33 112.9(3) . . ? C35 C20 C33 109.9(4) . . ? C22 C21 C5 116.3(4) . . ? C24 C23 C5 118.5(4) . . ? C26 C25 C10 115.7(4) . . ? C28 C27 C10 113.9(4) . . ? C30 C29 C15 115.5(4) . . ? C32 C31 C15 118.0(4) . . ? C34 C33 C20 112.7(4) . . ? C36 C35 C20 116.0(4) . . ? C37 Mo1 C39 85.0(2) . . ? C37 Mo1 C38 83.13(19) . . ? C39 Mo1 C38 87.9(2) . . ? C37 Mo1 C4 101.51(16) . . ? C39 Mo1 C4 125.79(18) . . ? C38 Mo1 C4 146.14(17) . . ? C37 Mo1 C3 118.58(17) . . ? C39 Mo1 C3 95.68(19) . . ? C38 Mo1 C3 158.19(17) . . ? C4 Mo1 C3 34.22(14) . . ? C37 Mo1 N1 115.66(15) . . ? C39 Mo1 N1 150.52(17) . . ? C38 Mo1 N1 114.12(16) . . ? C4 Mo1 N1 33.76(12) . . ? C3 Mo1 N1 56.60(13) . . ? C37 Mo1 C2 153.26(17) . . ? C39 Mo1 C2 95.76(18) . . ? C38 Mo1 C2 123.60(17) . . ? C4 Mo1 C2 56.68(14) . . ? C3 Mo1 C2 34.69(14) . . ? N1 Mo1 C2 56.15(13) . . ? C37 Mo1 C1 149.02(16) . . ? C39 Mo1 C1 124.88(18) . . ? C38 Mo1 C1 103.95(17) . . ? C4 Mo1 C1 56.22(14) . . ? C3 Mo1 C1 56.67(15) . . ? N1 Mo1 C1 33.80(12) . . ? C2 Mo1 C1 33.52(15) . . ? O1 C37 Mo1 177.7(4) . . ? C37 O1 Li2 145.8(4) . . ? O2 C38 Mo1 176.8(4) . . ? O3 C39 Mo1 177.5(5) . . ? C41 Mo2 C40 81.7(2) . . ? C41 Mo2 C42 84.9(3) . . ? C40 Mo2 C42 84.6(2) . . ? C41 Mo2 C12 100.7(2) . . ? C40 Mo2 C12 116.8(2) . . ? C42 Mo2 C12 158.4(2) . . ? C41 Mo2 C11 131.4(2) . . ? C40 Mo2 C11 102.40(18) . . ? C42 Mo2 C11 143.5(2) . . ? C12 Mo2 C11 34.03(15) . . ? C41 Mo2 C13 97.7(2) . . ? C40 Mo2 C13 150.9(2) . . ? C42 Mo2 C13 124.4(2) . . ? C12 Mo2 C13 34.49(16) . . ? C11 Mo2 C13 56.52(15) . . ? C41 Mo2 C14 125.0(2) . . ? C40 Mo2 C14 152.34(19) . . ? C42 Mo2 C14 103.4(2) . . ? C12 Mo2 C14 56.32(16) . . ? C11 Mo2 C14 55.85(14) . . ? C13 Mo2 C14 33.62(15) . . ? C41 Mo2 N3 153.5(2) . . ? C40 Mo2 N3 118.89(18) . . ? C42 Mo2 N3 112.0(2) . . ? C12 Mo2 N3 56.29(14) . . ? C11 Mo2 N3 33.62(12) . . ? C13 Mo2 N3 56.10(14) . . ? C14 Mo2 N3 33.53(13) . . ? O4 C40 Mo2 175.1(6) . . ? C40 O4 Li1 155.7(5) . . ? O5 C41 Mo2 178.8(6) . . ? C41 O5 Li1 156.9(6) . 4_545 ? O6 C42 Mo2 175.9(6) . . ? O8 Li1 O7 114.1(5) . . ? O8 Li1 O5 108.6(5) . 4 ? O7 Li1 O5 106.0(5) . 4 ? O8 Li1 O4 114.8(6) . . ? O7 Li1 O4 106.9(5) . . ? O5 Li1 O4 105.9(5) 4 . ? C46 O7 C43 106.9(7) . . ? C46 O7 Li1 121.9(7) . . ? C43 O7 Li1 118.8(6) . . ? O7 C43 C44 106.6(7) . . ? C45 C44 C43 107.9(7) . . ? C44 C45 C46 100.5(8) . . ? O7 C46 C45 104.6(7) . . ? C47 O8 C50 109.5(7) . . ? C47 O8 Li1 124.2(6) . . ? C50 O8 Li1 121.9(6) . . ? O8 C47 C48 104.5(8) . . ? C47 C48 C49 106.2(9) . . ? C50 C49 C48 106.6(9) . . ? C49 C50 O8 106.9(9) . . ? O9 Li2 O10 109.6(5) . . ? O9 Li2 O11 111.8(5) . . ? O10 Li2 O11 115.6(5) . . ? O9 Li2 O1 105.0(4) . . ? O10 Li2 O1 111.3(5) . . ? O11 Li2 O1 102.9(5) . . ? C54 O9 C51 107.8(4) . . ? C54 O9 Li2 119.7(4) . . ? C51 O9 Li2 126.8(4) . . ? O9 C51 C52 107.4(4) . . ? C51 C52 C53 103.8(4) . . ? C54 C53 C52 103.0(4) . . ? O9 C54 C53 104.4(4) . . ? C58 O10 C55 108.3(6) . . ? C58 O10 Li2 127.4(6) . . ? C55 O10 Li2 121.2(5) . . ? O10 C55 C56 108.7(7) . . ? C55 C56 C57 105.0(8) . . ? C56 C57 C58 104.5(8) . . ? O10 C58 C57 105.6(8) . . ? C59 O11 C62 108.7(7) . . ? C59 O11 Li2 122.8(6) . . ? C62 O11 Li2 115.3(5) . . ? C60 C59 O11 113.2(7) . . ? C59 C60 C61 87.3(8) . . ? C62 C61 C60 115.6(10) . . ? C61 C62 O11 96.7(9) . . ? C63 O12 C66 59.8(14) . . ? C64 C63 O12 141.5(16) . . ? C63 C64 C65 98.9(12) . . ? C66 C65 C64 81.6(11) . . ? C65 C66 O12 156.1(17) . . ? _refine_diff_density_max 1.661 _refine_diff_density_min -1.004 _refine_diff_density_rms 0.112 data_5 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H72 Li Mo4 N4 Ni O15, C16 H32 Li O4, C6 H6' _chemical_formula_sum 'C82 H110 Li2 Mo4 N4 Ni O19' _chemical_formula_weight 1912.09 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' 'Li' 'Li' -0.0003 0.0001 '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 27.300(6) _cell_length_b 17.269(2) _cell_length_c 18.076(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.17(2) _cell_angle_gamma 90.00 _cell_volume 8473(2) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used '413 spots from first image' _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3936 _exptl_absorpt_coefficient_mu 0.863 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'marresearch mar345 Imaging Plate Detector System' _diffrn_measurement_method ; phi scan (60 images with a delta phi of three degrees and an exposure time of three minutes per image) ; _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42857 _diffrn_reflns_av_R_equivalents 0.0380 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 25.03 _reflns_number_total 13785 _reflns_number_gt 11822 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'mar345, marresearch, release 1.2.11, 1999' _computing_cell_refinement 'marHKL, marresearch, release 1.9.1, 1997' _computing_data_reduction 'marHKL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL, release 5.1, 1997' _computing_publication_material '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^)+(0.0822P)^2^+10.7508P] 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 SHELXL _refine_ls_extinction_coef 0.00475(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 13785 _refine_ls_number_parameters 1010 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.1340 _refine_ls_wR_factor_gt 0.1273 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 Ni1 Ni 0.250585(17) -0.00033(3) 0.16475(3) 0.02555(13) Uani 1 1 d . . . N1 N 0.25758(11) 0.02509(18) 0.06575(18) 0.0271(7) Uani 1 1 d . . . N2 N 0.24411(12) -0.10555(19) 0.13925(18) 0.0283(7) Uani 1 1 d . . . N3 N 0.25626(11) -0.02588(18) 0.26625(17) 0.0265(7) Uani 1 1 d . . . N4 N 0.24413(12) 0.10435(18) 0.18833(18) 0.0270(7) Uani 1 1 d . . . C1 C 0.23224(14) 0.0828(2) 0.0245(2) 0.0287(8) Uani 1 1 d . . . C2 C 0.23703(15) 0.0716(2) -0.0506(2) 0.0311(9) Uani 1 1 d . . . H2 H 0.2229 0.1024 -0.0910 0.037 Uiso 1 1 calc R . . C3 C 0.26721(15) 0.0053(2) -0.0551(2) 0.0309(9) Uani 1 1 d . . . H3 H 0.2774 -0.0159 -0.0995 0.037 Uiso 1 1 calc R . . C4 C 0.27952(14) -0.0238(2) 0.0165(2) 0.0283(8) Uani 1 1 d . . . C5 C 0.30479(15) -0.0990(2) 0.0429(2) 0.0309(9) Uani 1 1 d . . . C6 C 0.27077(14) -0.1440(2) 0.0879(2) 0.0298(8) Uani 1 1 d . . . C7 C 0.26632(15) -0.2237(2) 0.0989(2) 0.0333(9) Uani 1 1 d . . . H7 H 0.2807 -0.2635 0.0722 0.040 Uiso 1 1 calc R . . C8 C 0.23602(15) -0.2340(2) 0.1581(2) 0.0316(9) Uani 1 1 d . . . H8 H 0.2265 -0.2821 0.1776 0.038 Uiso 1 1 calc R . . C9 C 0.22300(14) -0.1612(2) 0.1819(2) 0.0298(9) Uani 1 1 d . . . C10 C 0.19709(15) -0.1380(2) 0.2490(2) 0.0310(9) Uani 1 1 d . . . C11 C 0.23066(14) -0.0848(2) 0.2979(2) 0.0300(8) Uani 1 1 d . . . C12 C 0.23527(15) -0.0730(2) 0.3752(2) 0.0324(9) Uani 1 1 d . . . H12 H 0.2212 -0.1040 0.4108 0.039 Uiso 1 1 calc R . . C13 C 0.26492(15) -0.0063(2) 0.3901(2) 0.0317(9) Uani 1 1 d . . . H13 H 0.2745 0.0151 0.4379 0.038 Uiso 1 1 calc R . . C14 C 0.27755(14) 0.0226(2) 0.3231(2) 0.0276(8) Uani 1 1 d . . . C15 C 0.30278(14) 0.0987(2) 0.3062(2) 0.0283(8) Uani 1 1 d . . . C16 C 0.26938(13) 0.1435(2) 0.2488(2) 0.0286(8) Uani 1 1 d . . . C17 C 0.26518(14) 0.2230(2) 0.2367(2) 0.0292(8) Uani 1 1 d . . . H17 H 0.2793 0.2627 0.2686 0.035 Uiso 1 1 calc R . . C18 C 0.23558(14) 0.2335(2) 0.1673(2) 0.0320(9) Uani 1 1 d . . . H18 H 0.2260 0.2818 0.1451 0.038 Uiso 1 1 calc R . . C19 C 0.22331(14) 0.1607(2) 0.1379(2) 0.0286(8) Uani 1 1 d . . . C20 C 0.19817(14) 0.1376(2) 0.0616(2) 0.0297(8) Uani 1 1 d . . . C21 C 0.31666(16) -0.1473(3) -0.0252(2) 0.0360(9) Uani 1 1 d . . . H21A H 0.3228 -0.2015 -0.0091 0.043 Uiso 1 1 calc R . . H21B H 0.2873 -0.1472 -0.0625 0.043 Uiso 1 1 calc R . . C22 C 0.36089(18) -0.1189(3) -0.0627(3) 0.0455(11) Uani 1 1 d . . . H22A H 0.3565 -0.0640 -0.0755 0.068 Uiso 1 1 calc R . . H22B H 0.3635 -0.1490 -0.1081 0.068 Uiso 1 1 calc R . . H22C H 0.3910 -0.1255 -0.0286 0.068 Uiso 1 1 calc R . . C23 C 0.35259(15) -0.0845(3) 0.0965(2) 0.0351(9) Uani 1 1 d . . . H23A H 0.3757 -0.0536 0.0698 0.042 Uiso 1 1 calc R . . H23B H 0.3439 -0.0531 0.1391 0.042 Uiso 1 1 calc R . . C24 C 0.37912(17) -0.1572(3) 0.1268(3) 0.0428(11) Uani 1 1 d . . . H24A H 0.3575 -0.1866 0.1564 0.064 Uiso 1 1 calc R . . H24B H 0.4092 -0.1426 0.1582 0.064 Uiso 1 1 calc R . . H24C H 0.3877 -0.1891 0.0853 0.064 Uiso 1 1 calc R . . C25 C 0.18526(17) -0.2105(3) 0.2939(2) 0.0368(10) Uani 1 1 d . . . H25A H 0.2153 -0.2430 0.3017 0.044 Uiso 1 1 calc R . . H25B H 0.1771 -0.1937 0.3435 0.044 Uiso 1 1 calc R . . C26 C 0.14273(18) -0.2607(3) 0.2577(3) 0.0444(11) Uani 1 1 d . . . H26A H 0.1113 -0.2343 0.2618 0.067 Uiso 1 1 calc R . . H26B H 0.1428 -0.3108 0.2832 0.067 Uiso 1 1 calc R . . H26C H 0.1469 -0.2689 0.2051 0.067 Uiso 1 1 calc R . . C27 C 0.14928(14) -0.0907(3) 0.2254(2) 0.0323(9) Uani 1 1 d . . . H27A H 0.1581 -0.0452 0.1963 0.039 Uiso 1 1 calc R . . H27B H 0.1267 -0.1234 0.1921 0.039 Uiso 1 1 calc R . . C28 C 0.12181(16) -0.0626(3) 0.2893(3) 0.0429(11) Uani 1 1 d . . . H28A H 0.1140 -0.1068 0.3199 0.064 Uiso 1 1 calc R . . H28B H 0.0912 -0.0369 0.2693 0.064 Uiso 1 1 calc R . . H28C H 0.1425 -0.0259 0.3199 0.064 Uiso 1 1 calc R . . C29 C 0.35148(15) 0.0849(2) 0.2707(2) 0.0320(9) Uani 1 1 d . . . H29A H 0.3742 0.0549 0.3062 0.038 Uiso 1 1 calc R . . H29B H 0.3440 0.0528 0.2255 0.038 Uiso 1 1 calc R . . C30 C 0.37800(16) 0.1582(3) 0.2494(3) 0.0396(10) Uani 1 1 d . . . H30A H 0.3567 0.1871 0.2120 0.059 Uiso 1 1 calc R . . H30B H 0.4085 0.1439 0.2288 0.059 Uiso 1 1 calc R . . H30C H 0.3858 0.1905 0.2937 0.059 Uiso 1 1 calc R . . C31 C 0.31250(16) 0.1465(2) 0.3784(2) 0.0326(9) Uani 1 1 d . . . H31A H 0.3183 0.2010 0.3648 0.039 Uiso 1 1 calc R . . H31B H 0.2825 0.1453 0.4046 0.039 Uiso 1 1 calc R . . C32 C 0.35606(16) 0.1192(3) 0.4322(2) 0.0396(10) Uani 1 1 d . . . H32A H 0.3536 0.0632 0.4398 0.059 Uiso 1 1 calc R . . H32B H 0.3557 0.1460 0.4799 0.059 Uiso 1 1 calc R . . H32C H 0.3869 0.1309 0.4113 0.059 Uiso 1 1 calc R . . C33 C 0.18774(16) 0.2109(3) 0.0135(2) 0.0369(10) Uani 1 1 d . . . H33A H 0.2180 0.2430 0.0170 0.044 Uiso 1 1 calc R . . H33B H 0.1802 0.1951 -0.0391 0.044 Uiso 1 1 calc R . . C34 C 0.14526(17) 0.2606(3) 0.0356(3) 0.0444(11) Uani 1 1 d . . . H34A H 0.1141 0.2330 0.0233 0.067 Uiso 1 1 calc R . . H34B H 0.1444 0.3098 0.0085 0.067 Uiso 1 1 calc R . . H34C H 0.1501 0.2708 0.0892 0.067 Uiso 1 1 calc R . . C35 C 0.14988(15) 0.0921(3) 0.0689(2) 0.0336(9) Uani 1 1 d . . . H35A H 0.1579 0.0465 0.1011 0.040 Uiso 1 1 calc R . . H35B H 0.1275 0.1256 0.0943 0.040 Uiso 1 1 calc R . . C36 C 0.12235(17) 0.0641(3) -0.0041(2) 0.0446(11) Uani 1 1 d . . . H36A H 0.1146 0.1085 -0.0372 0.067 Uiso 1 1 calc R . . H36B H 0.0917 0.0385 0.0059 0.067 Uiso 1 1 calc R . . H36C H 0.1430 0.0274 -0.0281 0.067 Uiso 1 1 calc R . . Mo1 Mo 0.316369(13) 0.10365(2) 0.01147(2) 0.03089(12) Uani 1 1 d . . . C37 C 0.34539(16) 0.1483(3) -0.0704(3) 0.0392(10) Uani 1 1 d . . . O1 O 0.36266(14) 0.17545(19) -0.1211(2) 0.0514(9) Uani 1 1 d . . . C38 C 0.32283(16) 0.2062(3) 0.0547(3) 0.0408(11) Uani 1 1 d . . . O2 O 0.32717(13) 0.2679(2) 0.0796(2) 0.0525(9) Uani 1 1 d . . . C39 C 0.38313(19) 0.0889(3) 0.0573(3) 0.0458(11) Uani 1 1 d . . . O3 O 0.42395(13) 0.0816(2) 0.0840(2) 0.0625(10) Uani 1 1 d . . . Mo2 Mo 0.187097(13) -0.17724(2) 0.053102(19) 0.03107(12) Uani 1 1 d . . . C40 C 0.11779(19) -0.1548(3) 0.0548(2) 0.0445(11) Uani 1 1 d . . . O4 O 0.07566(13) -0.1438(3) 0.0545(2) 0.0639(10) Uani 1 1 d . . . C41 C 0.16376(16) -0.2712(3) 0.0055(2) 0.0383(10) Uani 1 1 d . . . O5 O 0.15039(13) -0.32946(19) -0.02300(19) 0.0505(9) Uani 1 1 d . . . C42 C 0.17888(17) -0.1319(3) -0.0451(3) 0.0429(11) Uani 1 1 d . . . O6 O 0.17341(14) -0.1056(2) -0.10556(19) 0.0583(10) Uani 1 1 d . . . Mo3 Mo 0.315467(13) -0.10346(2) 0.34018(2) 0.03122(12) Uani 1 1 d . . . C43 C 0.34668(18) -0.1434(3) 0.4324(3) 0.0438(11) Uani 1 1 d . . . O7 O 0.36585(16) -0.1677(2) 0.4892(2) 0.0624(11) Uani 1 1 d . . . C44 C 0.32384(17) -0.2069(3) 0.3011(3) 0.0431(11) Uani 1 1 d . . . O8 O 0.33028(15) -0.2685(2) 0.2791(2) 0.0608(10) Uani 1 1 d . . . C45 C 0.38082(18) -0.0874(3) 0.3160(3) 0.0440(11) Uani 1 1 d . . . O9 O 0.42178(12) -0.0780(2) 0.3013(2) 0.0591(10) Uani 1 1 d . . . Mo4 Mo 0.185579(13) 0.17410(2) 0.254152(19) 0.02989(12) Uani 1 1 d . . . C46 C 0.11870(18) 0.1405(3) 0.2291(2) 0.0423(11) Uani 1 1 d . . . O10 O 0.07743(13) 0.1201(2) 0.2153(2) 0.0601(10) Uani 1 1 d . . . C47 C 0.17729(16) 0.1303(3) 0.3500(3) 0.0388(10) Uani 1 1 d . . . O11 O 0.17173(14) 0.1040(2) 0.40870(19) 0.0523(9) Uani 1 1 d . . . C48 C 0.15849(16) 0.2666(3) 0.2922(2) 0.0378(10) Uani 1 1 d . . . O12 O 0.14245(13) 0.32402(19) 0.3142(2) 0.0511(9) Uani 1 1 d . . . Li1 Li 0.4924(3) -0.0777(6) 0.3095(5) 0.061(2) Uani 1 1 d . . . O13 O 0.51928(14) -0.0673(2) 0.2176(2) 0.0644(10) Uani 1 1 d . . . C49 C 0.5268(3) 0.0030(4) 0.1770(4) 0.093(2) Uani 1 1 d . . . H49A H 0.5545 0.0332 0.2025 0.112 Uiso 1 1 calc R . . H49B H 0.4968 0.0354 0.1731 0.112 Uiso 1 1 calc R . . C50 C 0.5385(3) -0.0216(5) 0.1008(4) 0.090(2) Uani 1 1 d . . . H50A H 0.5239 0.0146 0.0620 0.108 Uiso 1 1 calc R . . H50B H 0.5745 -0.0246 0.0985 0.108 Uiso 1 1 calc R . . C51 C 0.5156(3) -0.0982(5) 0.0922(4) 0.095(3) Uani 1 1 d . . . H51A H 0.5310 -0.1300 0.0555 0.114 Uiso 1 1 calc R . . H51B H 0.4798 -0.0944 0.0771 0.114 Uiso 1 1 calc R . . C52 C 0.5261(3) -0.1312(4) 0.1703(4) 0.082(2) Uani 1 1 d . . . H52A H 0.5030 -0.1736 0.1785 0.098 Uiso 1 1 calc R . . H52B H 0.5603 -0.1511 0.1789 0.098 Uiso 1 1 calc R . . O14 O 0.50786(17) -0.1795(3) 0.3437(3) 0.0916(16) Uani 1 1 d . . . C53 C 0.5541(2) -0.1977(5) 0.3846(4) 0.083(2) Uani 1 1 d . . . H53A H 0.5736 -0.1500 0.3962 0.100 Uiso 1 1 calc R . . H53B H 0.5733 -0.2331 0.3557 0.100 Uiso 1 1 calc R . . C54 C 0.5422(2) -0.2346(4) 0.4521(4) 0.0746(18) Uani 1 1 d . . . H54A H 0.5404 -0.1962 0.4923 0.089 Uiso 1 1 calc R . . H54B H 0.5671 -0.2743 0.4690 0.089 Uiso 1 1 calc R . . C55 C 0.4920(3) -0.2717(5) 0.4301(5) 0.097(2) Uani 1 1 d . . . H55A H 0.4951 -0.3286 0.4262 0.116 Uiso 1 1 calc R . . H55B H 0.4690 -0.2597 0.4673 0.116 Uiso 1 1 calc R . . C56 C 0.4747(3) -0.2390(6) 0.3596(6) 0.130(4) Uani 1 1 d . . . H56A H 0.4733 -0.2793 0.3205 0.156 Uiso 1 1 calc R . . H56B H 0.4412 -0.2174 0.3610 0.156 Uiso 1 1 calc R . . O15 O 0.51731(16) 0.0056(3) 0.3724(3) 0.0960(17) Uani 1 1 d . . . C57 C 0.5668(2) 0.0367(5) 0.3746(4) 0.088(2) Uani 1 1 d . . . H57A H 0.5856 0.0092 0.3387 0.105 Uiso 1 1 calc R . . H57B H 0.5846 0.0311 0.4250 0.105 Uiso 1 1 calc R . . C58 C 0.5610(4) 0.1202(5) 0.3542(6) 0.124(4) Uani 1 1 d . . . H58A H 0.5886 0.1516 0.3784 0.148 Uiso 1 1 calc R . . H58B H 0.5589 0.1276 0.2996 0.148 Uiso 1 1 calc R . . C59 C 0.5139(5) 0.1403(9) 0.3833(10) 0.185(6) Uani 1 1 d . . . H59A H 0.5202 0.1692 0.4306 0.222 Uiso 1 1 calc R . . H59B H 0.4935 0.1730 0.3470 0.222 Uiso 1 1 calc R . . C60 C 0.4884(3) 0.0672(8) 0.3953(8) 0.172(7) Uani 1 1 d . . . H60A H 0.4839 0.0614 0.4486 0.207 Uiso 1 1 calc R . . H60B H 0.4556 0.0668 0.3662 0.207 Uiso 1 1 calc R . . Li2 Li 0.0395(3) -0.4889(5) 0.1689(5) 0.054(2) Uani 1 1 d . . . O16 O 0.01143(12) -0.39846(19) 0.11863(19) 0.0462(8) Uani 1 1 d . . . C61 C -0.04047(19) -0.3810(4) 0.1102(3) 0.0602(14) Uani 1 1 d . . . H61A H -0.0574 -0.4096 0.1476 0.072 Uiso 1 1 calc R . . H61B H -0.0556 -0.3957 0.0599 0.072 Uiso 1 1 calc R . . C62 C -0.0445(3) -0.2949(4) 0.1218(5) 0.083(2) Uani 1 1 d . . . H62A H -0.0599 -0.2697 0.0759 0.100 Uiso 1 1 calc R . . H62B H -0.0648 -0.2839 0.1628 0.100 Uiso 1 1 calc R . . C63 C 0.0030(3) -0.2677(5) 0.1395(8) 0.161(5) Uani 1 1 d . . . H63A H 0.0074 -0.2514 0.1923 0.193 Uiso 1 1 calc R . . H63B H 0.0084 -0.2219 0.1084 0.193 Uiso 1 1 calc R . . C64 C 0.0388(2) -0.3272(3) 0.1271(4) 0.0620(15) Uani 1 1 d . . . H64A H 0.0548 -0.3159 0.0817 0.074 Uiso 1 1 calc R . . H64B H 0.0645 -0.3305 0.1700 0.074 Uiso 1 1 calc R . . O17 O 0.03245(14) -0.4885(2) 0.2728(2) 0.0549(9) Uani 1 1 d . . . C65 C 0.0203(2) -0.5517(3) 0.3192(3) 0.0625(15) Uani 1 1 d . . . H65A H 0.0502 -0.5812 0.3379 0.075 Uiso 1 1 calc R . . H65B H -0.0034 -0.5874 0.2915 0.075 Uiso 1 1 calc R . . C66 C -0.0023(2) -0.5136(4) 0.3822(3) 0.0686(17) Uani 1 1 d . . . H66A H -0.0380 -0.5052 0.3693 0.082 Uiso 1 1 calc R . . H66B H 0.0028 -0.5453 0.4280 0.082 Uiso 1 1 calc R . . C67 C 0.0244(3) -0.4384(4) 0.3923(3) 0.0712(17) Uani 1 1 d . . . H67A H 0.0526 -0.4428 0.4314 0.085 Uiso 1 1 calc R . . H67B H 0.0021 -0.3972 0.4065 0.085 Uiso 1 1 calc R . . C68 C 0.0421(2) -0.4208(4) 0.3184(4) 0.0711(17) Uani 1 1 d . . . H68A H 0.0244 -0.3755 0.2952 0.085 Uiso 1 1 calc R . . H68B H 0.0778 -0.4092 0.3247 0.085 Uiso 1 1 calc R . . O18 O 0.01703(14) -0.5884(2) 0.1292(2) 0.0620(10) Uani 1 1 d . . . C69 C -0.0260(2) -0.6126(3) 0.0831(3) 0.0561(13) Uani 1 1 d . . . H69A H -0.0217 -0.6052 0.0299 0.067 Uiso 1 1 calc R . . H69B H -0.0551 -0.5828 0.0948 0.067 Uiso 1 1 calc R . . C70 C -0.0320(2) -0.6972(4) 0.1003(4) 0.0749(18) Uani 1 1 d . . . H70A H -0.0542 -0.7044 0.1395 0.090 Uiso 1 1 calc R . . H70B H -0.0453 -0.7261 0.0553 0.090 Uiso 1 1 calc R . . C71 C 0.0177(3) -0.7224(5) 0.1257(6) 0.120(4) Uani 1 1 d . . . H71A H 0.0172 -0.7581 0.1685 0.144 Uiso 1 1 calc R . . H71B H 0.0321 -0.7500 0.0853 0.144 Uiso 1 1 calc R . . C72 C 0.0465(2) -0.6548(4) 0.1476(5) 0.082(2) Uani 1 1 d . . . H72A H 0.0568 -0.6560 0.2018 0.098 Uiso 1 1 calc R . . H72B H 0.0764 -0.6534 0.1212 0.098 Uiso 1 1 calc R . . O19 O 0.10819(13) -0.4840(3) 0.1567(2) 0.0671(11) Uani 1 1 d . . . C73 C 0.1249(2) -0.4882(5) 0.0833(4) 0.085(2) Uani 1 1 d . . . H73A H 0.1173 -0.4394 0.0558 0.102 Uiso 1 1 calc R . . H73B H 0.1084 -0.5314 0.0545 0.102 Uiso 1 1 calc R . . C74 C 0.1781(3) -0.5009(6) 0.0942(4) 0.097(3) Uani 1 1 d . . . H74A H 0.1963 -0.4514 0.0923 0.116 Uiso 1 1 calc R . . H74B H 0.1887 -0.5365 0.0560 0.116 Uiso 1 1 calc R . . C75 C 0.1863(2) -0.5374(5) 0.1723(5) 0.090(2) Uani 1 1 d . . . H75A H 0.1807 -0.5940 0.1702 0.108 Uiso 1 1 calc R . . H75B H 0.2200 -0.5270 0.1962 0.108 Uiso 1 1 calc R . . C76 C 0.1492(2) -0.4982(4) 0.2120(4) 0.0656(15) Uani 1 1 d . . . H76A H 0.1391 -0.5315 0.2522 0.079 Uiso 1 1 calc R . . H76B H 0.1623 -0.4489 0.2339 0.079 Uiso 1 1 calc R . . C77 C 0.32382(19) 0.4194(3) 0.1879(3) 0.0514(12) Uani 1 1 d . . . H77 H 0.3279 0.3651 0.1943 0.062 Uiso 1 1 calc R . . C78 C 0.3292(2) 0.4678(3) 0.2484(3) 0.0570(13) Uani 1 1 d . . . H78 H 0.3364 0.4469 0.2970 0.068 Uiso 1 1 calc R . . C79 C 0.3240(2) 0.5474(3) 0.2387(3) 0.0613(15) Uani 1 1 d . . . H79 H 0.3273 0.5809 0.2807 0.074 Uiso 1 1 calc R . . C80 C 0.3141(2) 0.5773(3) 0.1690(3) 0.0542(13) Uani 1 1 d . . . H80 H 0.3115 0.6318 0.1623 0.065 Uiso 1 1 calc R . . C81 C 0.3081(2) 0.5290(3) 0.1085(3) 0.0547(13) Uani 1 1 d . . . H81 H 0.3007 0.5503 0.0601 0.066 Uiso 1 1 calc R . . C82 C 0.3124(2) 0.4504(3) 0.1172(3) 0.0549(13) Uani 1 1 d . . . H82 H 0.3076 0.4172 0.0751 0.066 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 Ni1 0.0328(3) 0.0221(3) 0.0218(3) -0.0002(2) 0.00318(19) -0.00115(19) N1 0.0308(17) 0.0219(17) 0.0287(17) -0.0009(14) 0.0038(13) -0.0009(12) N2 0.0330(18) 0.0290(19) 0.0223(16) -0.0014(14) 0.0002(13) -0.0027(13) N3 0.0287(16) 0.0238(17) 0.0265(17) 0.0015(14) 0.0005(12) -0.0001(12) N4 0.0306(17) 0.0269(18) 0.0238(16) 0.0000(14) 0.0044(13) -0.0014(12) C1 0.030(2) 0.028(2) 0.028(2) -0.0002(18) 0.0048(15) -0.0023(16) C2 0.040(2) 0.029(2) 0.025(2) 0.0026(18) 0.0020(16) -0.0018(16) C3 0.041(2) 0.027(2) 0.026(2) -0.0039(18) 0.0041(16) -0.0049(16) C4 0.035(2) 0.024(2) 0.027(2) -0.0025(17) 0.0046(15) -0.0028(15) C5 0.039(2) 0.024(2) 0.030(2) -0.0020(17) 0.0059(17) 0.0027(16) C6 0.034(2) 0.028(2) 0.027(2) -0.0006(18) 0.0004(15) -0.0008(16) C7 0.039(2) 0.029(2) 0.031(2) -0.0002(18) -0.0008(16) 0.0043(17) C8 0.040(2) 0.026(2) 0.028(2) 0.0017(18) -0.0021(16) -0.0016(16) C9 0.035(2) 0.031(2) 0.0221(19) 0.0026(17) -0.0013(15) -0.0049(16) C10 0.037(2) 0.029(2) 0.028(2) 0.0020(18) 0.0047(16) -0.0053(17) C11 0.032(2) 0.029(2) 0.029(2) -0.0015(18) 0.0007(15) -0.0010(16) C12 0.039(2) 0.031(2) 0.027(2) 0.0013(18) 0.0045(16) -0.0008(17) C13 0.038(2) 0.035(2) 0.0217(19) -0.0038(18) 0.0009(15) -0.0020(17) C14 0.030(2) 0.025(2) 0.028(2) -0.0018(17) 0.0009(15) 0.0011(15) C15 0.033(2) 0.028(2) 0.023(2) -0.0020(17) 0.0011(15) -0.0032(15) C16 0.0271(19) 0.031(2) 0.028(2) -0.0001(18) 0.0038(15) -0.0007(15) C17 0.033(2) 0.026(2) 0.029(2) -0.0034(18) 0.0059(15) -0.0048(15) C18 0.035(2) 0.027(2) 0.035(2) 0.0049(18) 0.0097(16) 0.0024(16) C19 0.032(2) 0.029(2) 0.026(2) 0.0007(17) 0.0084(15) 0.0014(15) C20 0.034(2) 0.030(2) 0.026(2) 0.0015(18) 0.0027(15) 0.0033(16) C21 0.046(2) 0.032(2) 0.031(2) -0.003(2) 0.0066(17) 0.0048(18) C22 0.054(3) 0.051(3) 0.033(2) -0.006(2) 0.011(2) 0.008(2) C23 0.035(2) 0.035(2) 0.036(2) -0.004(2) 0.0071(17) 0.0003(17) C24 0.043(3) 0.042(3) 0.043(3) 0.001(2) 0.0022(19) 0.011(2) C25 0.052(3) 0.031(2) 0.027(2) 0.0047(19) 0.0026(17) -0.0113(19) C26 0.057(3) 0.038(3) 0.039(2) 0.001(2) 0.005(2) -0.016(2) C27 0.032(2) 0.037(2) 0.028(2) 0.0020(19) 0.0014(16) -0.0049(17) C28 0.038(2) 0.051(3) 0.042(2) -0.004(2) 0.0112(19) -0.004(2) C29 0.034(2) 0.032(2) 0.030(2) -0.0044(19) 0.0019(16) -0.0009(17) C30 0.037(2) 0.039(3) 0.044(3) -0.001(2) 0.0079(19) -0.0072(18) C31 0.045(2) 0.029(2) 0.024(2) -0.0024(18) 0.0037(16) -0.0059(17) C32 0.044(3) 0.042(3) 0.031(2) -0.006(2) -0.0014(18) -0.0095(19) C33 0.048(3) 0.032(2) 0.031(2) 0.004(2) 0.0052(18) 0.0069(18) C34 0.051(3) 0.042(3) 0.040(2) 0.009(2) 0.003(2) 0.017(2) C35 0.035(2) 0.036(2) 0.029(2) 0.0028(19) 0.0012(16) -0.0009(17) C36 0.043(3) 0.054(3) 0.035(2) -0.003(2) -0.0019(19) -0.004(2) Mo1 0.0379(2) 0.0271(2) 0.0286(2) -0.00016(15) 0.00789(14) -0.00196(13) C37 0.045(3) 0.029(2) 0.044(3) -0.004(2) 0.008(2) 0.0048(18) O1 0.072(2) 0.0374(19) 0.050(2) 0.0104(16) 0.0342(18) 0.0063(15) C38 0.041(2) 0.044(3) 0.040(2) 0.001(2) 0.0146(19) -0.005(2) O2 0.066(2) 0.037(2) 0.059(2) -0.0139(18) 0.0264(17) -0.0152(16) C39 0.055(3) 0.039(3) 0.045(3) -0.001(2) 0.010(2) -0.004(2) O3 0.044(2) 0.070(3) 0.071(3) 0.005(2) -0.0071(18) -0.0047(18) Mo2 0.0393(2) 0.0273(2) 0.0260(2) -0.00190(15) 0.00103(14) -0.00209(14) C40 0.060(3) 0.043(3) 0.029(2) -0.005(2) 0.000(2) 0.002(2) O4 0.044(2) 0.094(3) 0.052(2) -0.004(2) 0.0000(16) 0.015(2) C41 0.039(2) 0.048(3) 0.028(2) 0.006(2) 0.0036(17) 0.002(2) O5 0.068(2) 0.0370(19) 0.047(2) -0.0107(16) 0.0063(16) -0.0142(16) C42 0.046(3) 0.039(3) 0.042(3) 0.000(2) -0.0005(19) -0.008(2) O6 0.078(3) 0.063(3) 0.0308(18) 0.0091(17) -0.0077(16) -0.0166(18) Mo3 0.0376(2) 0.0270(2) 0.0281(2) 0.00127(15) -0.00117(14) -0.00051(13) C43 0.059(3) 0.026(2) 0.045(3) -0.006(2) -0.002(2) -0.005(2) O7 0.091(3) 0.048(2) 0.041(2) 0.0112(18) -0.0238(19) 0.0004(19) C44 0.049(3) 0.039(3) 0.037(2) 0.003(2) -0.0117(19) -0.001(2) O8 0.092(3) 0.0294(19) 0.056(2) -0.0078(17) -0.0153(19) 0.0142(17) C45 0.053(3) 0.034(2) 0.045(3) -0.001(2) 0.001(2) 0.008(2) O9 0.0364(19) 0.061(2) 0.081(3) 0.002(2) 0.0119(17) 0.0044(16) Mo4 0.0335(2) 0.0294(2) 0.0271(2) -0.00150(15) 0.00493(14) 0.00047(13) C46 0.053(3) 0.045(3) 0.030(2) -0.003(2) 0.0078(19) -0.002(2) O10 0.042(2) 0.089(3) 0.050(2) -0.004(2) 0.0039(15) -0.0192(18) C47 0.039(2) 0.035(2) 0.043(3) -0.003(2) 0.0085(19) 0.0040(18) O11 0.066(2) 0.057(2) 0.0368(19) 0.0071(17) 0.0174(16) 0.0087(17) C48 0.039(2) 0.045(3) 0.030(2) 0.000(2) 0.0052(17) -0.0044(19) O12 0.066(2) 0.0377(19) 0.051(2) -0.0075(16) 0.0139(17) 0.0146(16) Li1 0.051(5) 0.076(7) 0.058(5) -0.007(5) 0.009(4) 0.009(4) O13 0.068(2) 0.070(3) 0.058(2) -0.004(2) 0.0202(18) 0.009(2) C49 0.140(7) 0.066(5) 0.070(5) 0.003(4) -0.006(4) 0.013(4) C50 0.086(5) 0.122(7) 0.063(4) 0.004(4) 0.012(3) -0.015(5) C51 0.083(5) 0.137(8) 0.067(4) -0.021(5) 0.019(4) -0.013(5) C52 0.090(5) 0.077(5) 0.084(5) -0.016(4) 0.033(4) 0.003(4) O14 0.062(3) 0.105(4) 0.105(4) 0.038(3) -0.005(3) 0.008(2) C53 0.052(4) 0.101(5) 0.095(5) 0.023(4) 0.004(3) 0.018(3) C54 0.059(4) 0.072(4) 0.090(5) -0.003(4) -0.006(3) -0.001(3) C55 0.072(5) 0.093(6) 0.121(6) 0.021(5) -0.009(4) -0.021(4) C56 0.098(6) 0.103(7) 0.172(10) 0.041(7) -0.062(6) -0.022(5) O15 0.051(2) 0.132(5) 0.105(4) -0.055(3) 0.005(2) 0.012(3) C57 0.053(4) 0.110(6) 0.097(5) -0.034(5) -0.008(3) 0.007(4) C58 0.126(8) 0.091(6) 0.140(8) -0.034(6) -0.047(6) 0.031(5) C59 0.134(11) 0.157(13) 0.272(19) -0.058(12) 0.056(11) 0.044(9) C60 0.070(6) 0.194(13) 0.254(15) -0.141(13) 0.020(7) 0.018(7) Li2 0.053(5) 0.049(5) 0.061(5) -0.003(4) 0.006(4) 0.002(4) O16 0.0424(18) 0.049(2) 0.0466(19) 0.0007(16) 0.0016(14) -0.0020(14) C61 0.041(3) 0.080(4) 0.058(3) -0.001(3) 0.001(2) -0.001(3) C62 0.074(4) 0.072(5) 0.102(5) 0.012(4) 0.003(4) 0.021(4) C63 0.106(7) 0.065(5) 0.324(17) -0.050(8) 0.081(9) -0.003(5) C64 0.055(3) 0.056(4) 0.076(4) -0.008(3) 0.007(3) -0.013(2) O17 0.069(2) 0.044(2) 0.052(2) 0.0008(17) 0.0066(17) -0.0064(16) C65 0.073(4) 0.051(3) 0.062(3) 0.011(3) -0.003(3) -0.010(3) C66 0.066(4) 0.089(5) 0.050(3) 0.016(3) -0.001(3) 0.002(3) C67 0.100(5) 0.061(4) 0.048(3) -0.003(3) -0.010(3) 0.018(3) C68 0.070(4) 0.063(4) 0.083(4) -0.022(4) 0.017(3) -0.024(3) O18 0.058(2) 0.053(2) 0.072(3) -0.011(2) -0.0098(19) 0.0082(17) C69 0.049(3) 0.066(4) 0.052(3) -0.005(3) 0.004(2) -0.002(2) C70 0.068(4) 0.061(4) 0.096(5) -0.008(4) 0.015(3) -0.008(3) C71 0.101(6) 0.059(5) 0.187(10) 0.020(5) -0.044(6) -0.002(4) C72 0.064(4) 0.055(4) 0.120(6) -0.014(4) -0.019(4) 0.014(3) O19 0.045(2) 0.083(3) 0.073(3) 0.014(2) 0.0054(18) 0.0119(19) C73 0.065(4) 0.117(6) 0.074(4) 0.017(4) 0.010(3) 0.004(4) C74 0.065(4) 0.141(8) 0.087(5) 0.003(5) 0.014(4) 0.021(4) C75 0.056(4) 0.103(6) 0.111(6) 0.005(5) 0.009(4) 0.021(4) C76 0.059(3) 0.064(4) 0.072(4) -0.002(3) -0.001(3) 0.005(3) C77 0.059(3) 0.034(3) 0.063(3) 0.000(3) 0.017(2) 0.000(2) C78 0.078(4) 0.047(3) 0.045(3) 0.009(3) 0.004(2) 0.006(3) C79 0.092(4) 0.043(3) 0.046(3) -0.009(3) -0.006(3) 0.008(3) C80 0.077(4) 0.038(3) 0.046(3) -0.001(3) -0.001(2) 0.009(2) C81 0.070(4) 0.053(3) 0.040(3) 0.002(3) 0.003(2) 0.000(3) C82 0.067(3) 0.049(3) 0.051(3) -0.016(3) 0.016(2) -0.006(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N4 1.870(3) . ? Ni1 N1 1.872(3) . ? Ni1 N3 1.877(3) . ? Ni1 N2 1.878(3) . ? N1 C1 1.385(5) . ? N1 C4 1.407(5) . ? N1 Mo1 2.391(3) . ? N2 C9 1.395(5) . ? N2 C6 1.407(5) . ? N2 Mo2 2.421(3) . ? N3 C11 1.392(5) . ? N3 C14 1.403(5) . ? N3 Mo3 2.394(3) . ? N4 C16 1.401(5) . ? N4 C19 1.411(5) . ? N4 Mo4 2.415(3) . ? C1 C2 1.392(5) . ? C1 C20 1.530(5) . ? C1 Mo1 2.361(4) . ? C2 C3 1.419(6) . ? C2 Mo1 2.395(4) . ? C3 C4 1.395(6) . ? C3 Mo1 2.406(4) . ? C4 C5 1.524(5) . ? C4 Mo1 2.425(4) . ? C5 C6 1.513(5) . ? C5 C21 1.550(6) . ? C5 C23 1.560(6) . ? C6 C7 1.397(6) . ? C6 Mo2 2.373(4) . ? C7 C8 1.432(6) . ? C7 Mo2 2.371(4) . ? C8 C9 1.388(6) . ? C8 Mo2 2.408(4) . ? C9 C10 1.522(6) . ? C9 Mo2 2.443(4) . ? C10 C11 1.514(5) . ? C10 C25 1.545(6) . ? C10 C27 1.560(6) . ? C11 C12 1.404(6) . ? C11 Mo3 2.381(4) . ? C12 C13 1.417(6) . ? C12 Mo3 2.402(4) . ? C13 C14 1.387(6) . ? C13 Mo3 2.409(4) . ? C14 C15 1.529(5) . ? C14 Mo3 2.416(4) . ? C15 C16 1.519(5) . ? C15 C31 1.543(5) . ? C15 C29 1.555(5) . ? C16 C17 1.393(6) . ? C16 Mo4 2.360(4) . ? C17 C18 1.429(6) . ? C17 Mo4 2.384(4) . ? C18 C19 1.392(6) . ? C18 Mo4 2.417(4) . ? C19 C20 1.527(5) . ? C19 Mo4 2.448(4) . ? C20 C33 1.544(6) . ? C20 C35 1.553(6) . ? C21 C22 1.528(6) . ? C23 C24 1.521(6) . ? C25 C26 1.537(6) . ? C27 C28 1.523(6) . ? C29 C30 1.528(6) . ? C31 C32 1.528(6) . ? C33 C34 1.529(6) . ? C35 C36 1.525(6) . ? Mo1 C37 1.914(5) . ? Mo1 C38 1.936(5) . ? Mo1 C39 1.936(5) . ? C37 O1 1.172(5) . ? C38 O2 1.159(6) . ? C39 O3 1.173(6) . ? Mo2 C41 1.913(5) . ? Mo2 C42 1.930(5) . ? Mo2 C40 1.935(5) . ? C40 O4 1.165(6) . ? C41 O5 1.171(5) . ? C42 O6 1.179(6) . ? Mo3 C45 1.902(5) . ? Mo3 C43 1.918(5) . ? Mo3 C44 1.943(5) . ? C43 O7 1.178(6) . ? C44 O8 1.157(6) . ? C45 O9 1.188(6) . ? O9 Li1 1.918(10) . ? Mo4 C48 1.919(5) . ? Mo4 C46 1.923(5) . ? Mo4 C47 1.925(5) . ? C46 O10 1.181(6) . ? C47 O11 1.179(5) . ? C48 O12 1.170(5) . ? Li1 O14 1.896(12) . ? Li1 O13 1.897(10) . ? Li1 O15 1.912(12) . ? O13 C52 1.420(8) . ? O13 C49 1.444(8) . ? C49 C50 1.506(10) . ? C50 C51 1.464(11) . ? C51 C52 1.519(11) . ? O14 C56 1.418(10) . ? O14 C53 1.427(7) . ? C53 C54 1.445(9) . ? C54 C55 1.526(9) . ? C55 C56 1.427(11) . ? O15 C60 1.412(10) . ? O15 C57 1.451(8) . ? C57 C58 1.494(11) . ? C58 C59 1.482(14) . ? C59 C60 1.469(18) . ? Li2 O17 1.908(10) . ? Li2 O19 1.914(10) . ? Li2 O16 1.924(10) . ? Li2 O18 1.936(10) . ? O16 C64 1.439(6) . ? O16 C61 1.440(6) . ? C61 C62 1.507(9) . ? C62 C63 1.383(10) . ? C63 C64 1.453(9) . ? O17 C65 1.438(6) . ? O17 C68 1.439(7) . ? C65 C66 1.504(9) . ? C66 C67 1.489(9) . ? C67 C68 1.498(9) . ? O18 C72 1.420(7) . ? O18 C69 1.427(6) . ? C69 C70 1.505(8) . ? C70 C71 1.450(10) . ? C71 C72 1.439(10) . ? O19 C76 1.439(7) . ? O19 C73 1.450(8) . ? C73 C74 1.462(9) . ? C74 C75 1.541(11) . ? C75 C76 1.467(9) . ? C77 C78 1.372(8) . ? C77 C82 1.390(8) . ? C78 C79 1.391(8) . ? C79 C80 1.362(8) . ? C80 C81 1.371(7) . ? C81 C82 1.370(8) . ? 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 N4 Ni1 N1 90.74(14) . . ? N4 Ni1 N3 90.25(14) . . ? N1 Ni1 N3 169.48(14) . . ? N4 Ni1 N2 169.26(14) . . ? N1 Ni1 N2 90.50(14) . . ? N3 Ni1 N2 90.47(14) . . ? C1 N1 C4 108.3(3) . . ? C1 N1 Ni1 125.9(3) . . ? C4 N1 Ni1 124.0(3) . . ? C1 N1 Mo1 71.9(2) . . ? C4 N1 Mo1 74.4(2) . . ? Ni1 N1 Mo1 131.84(16) . . ? C9 N2 C6 108.3(3) . . ? C9 N2 Ni1 124.3(3) . . ? C6 N2 Ni1 125.2(3) . . ? C9 N2 Mo2 74.2(2) . . ? C6 N2 Mo2 71.1(2) . . ? Ni1 N2 Mo2 133.61(16) . . ? C11 N3 C14 108.7(3) . . ? C11 N3 Ni1 125.6(3) . . ? C14 N3 Ni1 124.1(3) . . ? C11 N3 Mo3 72.5(2) . . ? C14 N3 Mo3 73.9(2) . . ? Ni1 N3 Mo3 131.08(16) . . ? C16 N4 C19 107.5(3) . . ? C16 N4 Ni1 126.4(3) . . ? C19 N4 Ni1 124.1(3) . . ? C16 N4 Mo4 70.8(2) . . ? C19 N4 Mo4 74.5(2) . . ? Ni1 N4 Mo4 132.70(15) . . ? N1 C1 C2 109.4(3) . . ? N1 C1 C20 120.1(3) . . ? C2 C1 C20 129.6(4) . . ? N1 C1 Mo1 74.2(2) . . ? C2 C1 Mo1 74.3(2) . . ? C20 C1 Mo1 126.4(3) . . ? C1 C2 C3 106.5(4) . . ? C1 C2 Mo1 71.7(2) . . ? C3 C2 Mo1 73.2(2) . . ? C4 C3 C2 108.7(4) . . ? C4 C3 Mo1 74.0(2) . . ? C2 C3 Mo1 72.4(2) . . ? C3 C4 N1 107.2(3) . . ? C3 C4 C5 130.8(4) . . ? N1 C4 C5 121.5(3) . . ? C3 C4 Mo1 72.5(2) . . ? N1 C4 Mo1 71.7(2) . . ? C5 C4 Mo1 127.6(3) . . ? C6 C5 C4 108.8(3) . . ? C6 C5 C21 110.1(3) . . ? C4 C5 C21 109.6(3) . . ? C6 C5 C23 105.6(3) . . ? C4 C5 C23 112.2(3) . . ? C21 C5 C23 110.4(3) . . ? C7 C6 N2 108.1(3) . . ? C7 C6 C5 130.6(4) . . ? N2 C6 C5 120.2(3) . . ? C7 C6 Mo2 72.8(2) . . ? N2 C6 Mo2 74.8(2) . . ? C5 C6 Mo2 127.7(3) . . ? C6 C7 C8 107.2(4) . . ? C6 C7 Mo2 73.0(2) . . ? C8 C7 Mo2 74.0(2) . . ? C9 C8 C7 107.9(4) . . ? C9 C8 Mo2 74.8(2) . . ? C7 C8 Mo2 71.1(2) . . ? C8 C9 N2 108.5(3) . . ? C8 C9 C10 129.9(4) . . ? N2 C9 C10 121.0(3) . . ? C8 C9 Mo2 72.0(2) . . ? N2 C9 Mo2 72.5(2) . . ? C10 C9 Mo2 128.1(3) . . ? C11 C10 C9 108.7(3) . . ? C11 C10 C25 109.5(3) . . ? C9 C10 C25 110.3(3) . . ? C11 C10 C27 106.2(3) . . ? C9 C10 C27 111.5(3) . . ? C25 C10 C27 110.6(3) . . ? N3 C11 C12 108.0(3) . . ? N3 C11 C10 120.2(3) . . ? C12 C11 C10 130.7(4) . . ? N3 C11 Mo3 73.6(2) . . ? C12 C11 Mo3 73.8(2) . . ? C10 C11 Mo3 127.7(3) . . ? C11 C12 C13 107.2(4) . . ? C11 C12 Mo3 72.1(2) . . ? C13 C12 Mo3 73.1(2) . . ? C14 C13 C12 108.5(4) . . ? C14 C13 Mo3 73.6(2) . . ? C12 C13 Mo3 72.6(2) . . ? C13 C14 N3 107.6(3) . . ? C13 C14 C15 130.0(4) . . ? N3 C14 C15 121.8(3) . . ? C13 C14 Mo3 73.0(2) . . ? N3 C14 Mo3 72.2(2) . . ? C15 C14 Mo3 127.1(3) . . ? C16 C15 C14 108.9(3) . . ? C16 C15 C31 109.9(3) . . ? C14 C15 C31 109.4(3) . . ? C16 C15 C29 105.8(3) . . ? C14 C15 C29 112.0(3) . . ? C31 C15 C29 110.7(3) . . ? C17 C16 N4 109.2(3) . . ? C17 C16 C15 130.0(4) . . ? N4 C16 C15 119.7(3) . . ? C17 C16 Mo4 73.9(2) . . ? N4 C16 Mo4 75.1(2) . . ? C15 C16 Mo4 126.8(3) . . ? C16 C17 C18 107.0(3) . . ? C16 C17 Mo4 72.0(2) . . ? C18 C17 Mo4 73.9(2) . . ? C19 C18 C17 108.1(4) . . ? C19 C18 Mo4 74.6(2) . . ? C17 C18 Mo4 71.4(2) . . ? C18 C19 N4 108.2(3) . . ? C18 C19 C20 130.4(4) . . ? N4 C19 C20 121.0(3) . . ? C18 C19 Mo4 72.1(2) . . ? N4 C19 Mo4 71.8(2) . . ? C20 C19 Mo4 127.6(3) . . ? C19 C20 C1 108.8(3) . . ? C19 C20 C33 109.4(3) . . ? C1 C20 C33 110.2(3) . . ? C19 C20 C35 111.0(3) . . ? C1 C20 C35 106.6(3) . . ? C33 C20 C35 110.9(3) . . ? C22 C21 C5 115.0(4) . . ? C24 C23 C5 115.2(4) . . ? C26 C25 C10 115.1(3) . . ? C28 C27 C10 115.1(3) . . ? C30 C29 C15 115.3(4) . . ? C32 C31 C15 115.1(4) . . ? C34 C33 C20 114.3(4) . . ? C36 C35 C20 115.5(4) . . ? C37 Mo1 C38 85.20(18) . . ? C37 Mo1 C39 86.3(2) . . ? C38 Mo1 C39 84.6(2) . . ? C37 Mo1 C1 128.78(17) . . ? C38 Mo1 C1 98.42(16) . . ? C39 Mo1 C1 144.90(17) . . ? C37 Mo1 N1 153.84(16) . . ? C38 Mo1 N1 112.92(14) . . ? C39 Mo1 N1 113.11(16) . . ? C1 Mo1 N1 33.87(12) . . ? C37 Mo1 C2 99.15(17) . . ? C38 Mo1 C2 116.04(17) . . ? C39 Mo1 C2 158.88(18) . . ? C1 Mo1 C2 34.04(13) . . ? N1 Mo1 C2 56.51(12) . . ? C37 Mo1 C3 98.78(17) . . ? C38 Mo1 C3 150.41(17) . . ? C39 Mo1 C3 124.78(18) . . ? C1 Mo1 C3 56.37(14) . . ? N1 Mo1 C3 56.06(12) . . ? C2 Mo1 C3 34.38(14) . . ? C37 Mo1 C4 127.03(16) . . ? C38 Mo1 C4 146.62(15) . . ? C39 Mo1 C4 103.90(17) . . ? C1 Mo1 C4 56.38(14) . . ? N1 Mo1 C4 33.95(12) . . ? C2 Mo1 C4 56.65(14) . . ? C3 Mo1 C4 33.56(13) . . ? O1 C37 Mo1 179.2(4) . . ? O2 C38 Mo1 178.8(4) . . ? O3 C39 Mo1 178.2(5) . . ? C41 Mo2 C42 85.97(19) . . ? C41 Mo2 C40 84.17(19) . . ? C42 Mo2 C40 85.2(2) . . ? C41 Mo2 C7 96.77(17) . . ? C42 Mo2 C7 118.01(17) . . ? C40 Mo2 C7 156.79(17) . . ? C41 Mo2 C6 126.06(16) . . ? C42 Mo2 C6 99.13(16) . . ? C40 Mo2 C6 149.55(17) . . ? C7 Mo2 C6 34.25(14) . . ? C41 Mo2 C8 98.02(16) . . ? C42 Mo2 C8 152.76(17) . . ? C40 Mo2 C8 121.96(17) . . ? C7 Mo2 C8 34.85(14) . . ? C6 Mo2 C8 56.86(14) . . ? C41 Mo2 N2 152.03(15) . . ? C42 Mo2 N2 112.78(15) . . ? C40 Mo2 N2 116.69(16) . . ? C7 Mo2 N2 56.55(13) . . ? C6 Mo2 N2 34.11(12) . . ? C8 Mo2 N2 55.75(13) . . ? C41 Mo2 C9 127.26(16) . . ? C42 Mo2 C9 145.60(16) . . ? C40 Mo2 C9 104.75(16) . . ? C7 Mo2 C9 56.50(14) . . ? C6 Mo2 C9 56.23(13) . . ? C8 Mo2 C9 33.23(14) . . ? N2 Mo2 C9 33.32(12) . . ? O4 C40 Mo2 177.5(4) . . ? O5 C41 Mo2 178.5(4) . . ? O6 C42 Mo2 178.6(4) . . ? C45 Mo3 C43 85.0(2) . . ? C45 Mo3 C44 84.3(2) . . ? C43 Mo3 C44 85.78(19) . . ? C45 Mo3 C11 144.11(17) . . ? C43 Mo3 C11 130.81(18) . . ? C44 Mo3 C11 99.00(16) . . ? C45 Mo3 N3 112.57(16) . . ? C43 Mo3 N3 153.80(17) . . ? C44 Mo3 N3 114.23(15) . . ? C11 Mo3 N3 33.89(12) . . ? C45 Mo3 C12 158.86(18) . . ? C43 Mo3 C12 100.49(18) . . ? C44 Mo3 C12 116.32(17) . . ? C11 Mo3 C12 34.13(13) . . ? N3 Mo3 C12 56.26(12) . . ? C45 Mo3 C13 125.02(17) . . ? C43 Mo3 C13 98.27(17) . . ? C44 Mo3 C13 150.58(17) . . ? C11 Mo3 C13 56.58(14) . . ? N3 Mo3 C13 55.92(12) . . ? C12 Mo3 C13 34.27(14) . . ? C45 Mo3 C14 103.82(17) . . ? C43 Mo3 C14 125.42(17) . . ? C44 Mo3 C14 147.93(16) . . ? C11 Mo3 C14 56.52(13) . . ? N3 Mo3 C14 33.91(12) . . ? C12 Mo3 C14 56.37(14) . . ? C13 Mo3 C14 33.41(13) . . ? O7 C43 Mo3 179.8(5) . . ? O8 C44 Mo3 177.8(4) . . ? O9 C45 Mo3 179.3(5) . . ? C45 O9 Li1 161.0(5) . . ? C48 Mo4 C46 86.73(19) . . ? C48 Mo4 C47 85.30(18) . . ? C46 Mo4 C47 83.85(19) . . ? C48 Mo4 C16 127.87(16) . . ? C46 Mo4 C16 145.36(17) . . ? C47 Mo4 C16 99.05(16) . . ? C48 Mo4 C17 98.29(16) . . ? C46 Mo4 C17 158.71(16) . . ? C47 Mo4 C17 117.07(16) . . ? C16 Mo4 C17 34.15(14) . . ? C48 Mo4 N4 153.24(15) . . ? C46 Mo4 N4 113.30(16) . . ? C47 Mo4 N4 113.27(15) . . ? C16 Mo4 N4 34.11(12) . . ? C17 Mo4 N4 56.66(12) . . ? C48 Mo4 C18 98.36(16) . . ? C46 Mo4 C18 124.30(16) . . ? C47 Mo4 C18 151.67(16) . . ? C16 Mo4 C18 56.67(13) . . ? C17 Mo4 C18 34.62(13) . . ? N4 Mo4 C18 56.06(12) . . ? C48 Mo4 C19 126.86(16) . . ? C46 Mo4 C19 104.23(16) . . ? C47 Mo4 C19 146.69(16) . . ? C16 Mo4 C19 56.25(13) . . ? C17 Mo4 C19 56.38(13) . . ? N4 Mo4 C19 33.71(12) . . ? C18 Mo4 C19 33.23(14) . . ? O10 C46 Mo4 178.6(4) . . ? O11 C47 Mo4 179.2(4) . . ? O12 C48 Mo4 178.5(4) . . ? O14 Li1 O13 106.3(5) . . ? O14 Li1 O15 116.8(6) . . ? O13 Li1 O15 107.7(6) . . ? O14 Li1 O9 102.1(5) . . ? O13 Li1 O9 114.3(5) . . ? O15 Li1 O9 109.8(5) . . ? C52 O13 C49 108.1(5) . . ? C52 O13 Li1 122.9(5) . . ? C49 O13 Li1 127.9(5) . . ? O13 C49 C50 106.5(6) . . ? C51 C50 C49 102.8(6) . . ? C50 C51 C52 101.8(6) . . ? O13 C52 C51 104.1(6) . . ? C56 O14 C53 106.5(6) . . ? C56 O14 Li1 127.8(6) . . ? C53 O14 Li1 121.7(5) . . ? O14 C53 C54 105.5(5) . . ? C53 C54 C55 104.0(6) . . ? C56 C55 C54 105.6(7) . . ? O14 C56 C55 108.1(6) . . ? C60 O15 C57 105.1(7) . . ? C60 O15 Li1 124.5(6) . . ? C57 O15 Li1 124.4(5) . . ? O15 C57 C58 106.1(6) . . ? C59 C58 C57 102.2(10) . . ? C60 C59 C58 107.1(10) . . ? O15 C60 C59 108.4(9) . . ? O17 Li2 O19 108.5(5) . . ? O17 Li2 O16 112.6(5) . . ? O19 Li2 O16 104.8(5) . . ? O17 Li2 O18 107.9(5) . . ? O19 Li2 O18 105.7(5) . . ? O16 Li2 O18 116.8(5) . . ? C64 O16 C61 109.1(4) . . ? C64 O16 Li2 117.9(4) . . ? C61 O16 Li2 123.8(4) . . ? O16 C61 C62 106.0(5) . . ? C63 C62 C61 106.8(6) . . ? C62 C63 C64 110.6(7) . . ? O16 C64 C63 105.7(5) . . ? C65 O17 C68 108.7(4) . . ? C65 O17 Li2 128.8(4) . . ? C68 O17 Li2 122.4(4) . . ? O17 C65 C66 104.4(5) . . ? C67 C66 C65 103.8(5) . . ? C66 C67 C68 105.6(5) . . ? O17 C68 C67 106.8(5) . . ? C72 O18 C69 108.0(4) . . ? C72 O18 Li2 118.8(4) . . ? C69 O18 Li2 133.2(4) . . ? O18 C69 C70 105.4(5) . . ? C71 C70 C69 103.8(5) . . ? C72 C71 C70 108.0(6) . . ? O18 C72 C71 108.2(5) . . ? C76 O19 C73 109.2(4) . . ? C76 O19 Li2 127.7(5) . . ? C73 O19 Li2 120.8(5) . . ? O19 C73 C74 106.9(6) . . ? C73 C74 C75 103.1(6) . . ? C76 C75 C74 102.7(6) . . ? O19 C76 C75 105.4(5) . . ? C78 C77 C82 119.6(5) . . ? C77 C78 C79 120.0(5) . . ? C80 C79 C78 119.9(5) . . ? C79 C80 C81 120.1(5) . . ? C82 C81 C80 120.7(5) . . ? C81 C82 C77 119.6(5) . . ? _refine_diff_density_max 1.526 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.159