# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Prof. Anthony Wedd' _publ_contact_author_address ; School of Chemistry The University of Melbourne Parkville Victoria 3052 Australia ; _publ_contact_author_email AGW@UNIMELB.EDU.AU _publ_section_title ; Facile assembly of hybrid materials containing polyoxometalates cluster anions and organic dye cations: Crystal structures and initial spectral characterization ; loop_ _publ_author_name 'Jingli Xie.' 'Anthony G. Wedd' data_1 _database_code_depnum_ccdc_archive 'CCDC 619194' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H72 Mo18 N12 O62 S2' _chemical_formula_weight 3936.50 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' S S 0.1246 0.1234 '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 39.565(3) _cell_length_b 19.4321(14) _cell_length_c 23.6601(17) _cell_angle_alpha 90.00 _cell_angle_beta 121.9190(10) _cell_angle_gamma 90.00 _cell_volume 15440.3(19) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 6 _cell_measurement_theta_max 12 _exptl_crystal_description cuboid _exptl_crystal_colour black-purple _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.693 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7584 _exptl_absorpt_coefficient_mu 1.509 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.685 _exptl_absorpt_correction_T_max 0.770 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39164 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -46 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 24.71 _reflns_number_total 13159 _reflns_number_gt 10964 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SMART (Siemens, 1996)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990) ; _refine_special_details ; The largest residul electron density peak is 3.96 e?^-3^, which is located at 3.41? from H37 atom; the deepest hole is -0.67 e?^-3^, which is located at 0.91 ? from Mo2 atom. 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^)+(0.1193P)^2^+450.5811P] 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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13159 _refine_ls_number_parameters 766 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.2139 _refine_ls_wR_factor_gt 0.2070 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 0.11012(2) 0.21380(5) 1.00534(4) 0.0273(2) Uani 1 1 d . . . Mo2 Mo 0.12972(2) 0.37095(4) 0.96495(4) 0.0222(2) Uani 1 1 d . . . Mo3 Mo 0.15292(2) 0.22325(4) 0.91088(4) 0.0248(2) Uani 1 1 d . . . Mo4 Mo 0.00660(2) 0.27388(4) 0.92879(4) 0.0244(2) Uani 1 1 d . . . Mo5 Mo 0.02189(2) 0.42694(4) 0.87200(4) 0.0196(2) Uani 1 1 d . . . Mo6 Mo 0.07893(2) 0.42526(4) 0.78916(4) 0.0213(2) Uani 1 1 d . . . Mo7 Mo 0.09335(2) 0.27332(4) 0.73061(4) 0.0225(2) Uani 1 1 d . . . Mo8 Mo 0.07239(2) 0.10855(4) 0.78624(4) 0.0267(2) Uani 1 1 d . . . Mo9 Mo 0.02613(3) 0.10893(4) 0.87451(4) 0.0283(2) Uani 1 1 d . . . S1 S 0.05178(6) 0.26978(11) 0.83382(10) 0.0165(4) Uani 1 1 d . . . O1 O 0.1271(2) 0.1826(4) 1.0825(3) 0.0385(18) Uani 1 1 d . . . O2 O 0.16212(18) 0.4333(3) 1.0128(3) 0.0272(15) Uani 1 1 d . . . O3 O 0.19869(19) 0.1928(4) 0.9339(3) 0.0311(16) Uani 1 1 d . . . O4 O 0.13285(18) 0.3078(3) 1.0266(3) 0.0235(14) Uani 1 1 d . . . O5 O 0.16566(17) 0.3093(3) 0.9559(3) 0.0223(13) Uani 1 1 d . . . O6 O 0.15018(18) 0.1924(3) 0.9901(3) 0.0242(14) Uani 1 1 d . . . O7 O 0.06114(18) 0.2637(3) 0.9852(3) 0.0242(14) Uani 1 1 d . . . O8 O 0.08086(17) 0.4034(3) 0.9399(3) 0.0212(13) Uani 1 1 d . . . O9 O 0.11657(17) 0.4018(3) 0.8752(3) 0.0203(13) Uani 1 1 d . . . O10 O 0.13629(18) 0.2645(3) 0.8317(3) 0.0240(14) Uani 1 1 d . . . O11 O 0.11926(18) 0.1484(3) 0.8669(3) 0.0252(14) Uani 1 1 d . . . O12 O 0.07628(18) 0.1470(3) 0.9489(3) 0.0273(14) Uani 1 1 d . . . O13 O 0.09159(17) 0.2699(3) 0.8970(3) 0.0190(13) Uani 1 1 d . . . O14 O 0.02387(16) 0.3057(3) 0.8465(3) 0.0174(12) Uani 1 1 d . . . O15 O 0.05526(17) 0.3055(3) 0.7828(3) 0.0182(12) Uani 1 1 d . . . O16 O 0.03944(18) 0.1988(3) 0.8143(3) 0.0218(13) Uani 1 1 d . . . O17 O -0.00870(19) 0.2646(4) 0.9829(3) 0.0316(16) Uani 1 1 d . . . O18 O 0.01223(17) 0.3722(3) 0.9290(3) 0.0217(13) Uani 1 1 d . . . O19 O 0.02316(18) 0.5065(3) 0.9025(3) 0.0282(15) Uani 1 1 d . . . O20 O 0.04225(17) 0.4404(3) 0.8168(3) 0.0185(12) Uani 1 1 d . . . O21 O 0.09300(19) 0.5048(3) 0.7836(3) 0.0277(15) Uani 1 1 d . . . O22 O 0.10082(17) 0.3705(3) 0.7512(3) 0.0203(13) Uani 1 1 d . . . O23 O 0.12524(19) 0.2568(4) 0.7056(3) 0.0302(15) Uani 1 1 d . . . O24 O 0.08029(18) 0.1860(3) 0.7430(3) 0.0239(14) Uani 1 1 d . . . O25 O 0.0964(2) 0.0427(4) 0.7760(4) 0.0386(18) Uani 1 1 d . . . O26 O 0.05544(19) 0.0694(3) 0.8400(3) 0.0286(15) Uani 1 1 d . . . O27 O 0.0219(2) 0.0426(4) 0.9161(3) 0.0404(18) Uani 1 1 d . . . O28 O 0.00336(18) 0.1866(3) 0.8947(3) 0.0249(14) Uani 1 1 d . . . O29 O -0.02885(17) 0.4231(3) 0.8026(3) 0.0206(13) Uani 1 1 d . . . O30 O 0.04667(18) 0.2892(3) 0.6520(3) 0.0235(14) Uani 1 1 d . . . O31 O 0.02183(19) 0.0994(4) 0.7092(3) 0.0289(15) Uani 1 1 d . . . N1 N 0.0384(3) 0.4593(6) 0.0504(4) 0.048(3) Uani 1 1 d . . . H1A H 0.0228 0.4901 0.0505 0.058 Uiso 1 1 calc R . . H1B H 0.0289 0.4273 0.0209 0.058 Uiso 1 1 calc R . . N2 N 0.2378(3) 0.5913(5) 0.4862(4) 0.044(2) Uani 1 1 d . . . H2A H 0.2592 0.6153 0.5081 0.053 Uiso 1 1 calc R . . H2B H 0.2212 0.5898 0.4991 0.053 Uiso 1 1 calc R . . N3 N 0.3181(3) 0.3605(5) 0.2055(4) 0.036(2) Uani 1 1 d . . . H3A H 0.3148 0.3638 0.1666 0.043 Uiso 1 1 calc R . . H3B H 0.3399 0.3437 0.2380 0.043 Uiso 1 1 calc R . . N4 N 0.2649(3) 0.2433(5) 0.9125(4) 0.039(2) Uani 1 1 d . . . H4A H 0.2491 0.2450 0.9270 0.047 Uiso 1 1 calc R . . H4B H 0.2879 0.2243 0.9362 0.047 Uiso 1 1 calc R . . N5 N 0.3236(3) 0.4928(8) 0.6100(6) 0.083(5) Uani 1 1 d . . . H5A H 0.3447 0.5124 0.6415 0.100 Uiso 1 1 calc R . . H5B H 0.3179 0.4954 0.5696 0.100 Uiso 1 1 calc R . . N6 N 0.0524(3) 0.3712(6) 0.4868(5) 0.056(3) Uani 1 1 d . . . H6A H 0.0376 0.3383 0.4858 0.068 Uiso 1 1 calc R . . H6B H 0.0417 0.4068 0.4619 0.068 Uiso 1 1 calc R . . C1 C 0.0779(3) 0.4614(6) 0.0967(4) 0.035(2) Uani 1 1 d . . . C2 C 0.0936(3) 0.5125(6) 0.1444(5) 0.034(2) Uani 1 1 d . . . H2 H 0.0773 0.5478 0.1430 0.041 Uiso 1 1 calc R . . C3 C 0.1331(3) 0.5114(5) 0.1937(4) 0.029(2) Uani 1 1 d . . . H3 H 0.1429 0.5453 0.2264 0.035 Uiso 1 1 calc R . . C4 C 0.1594(3) 0.4604(5) 0.1965(5) 0.028(2) Uani 1 1 d . . . C5 C 0.1427(3) 0.4107(6) 0.1455(5) 0.034(2) Uani 1 1 d . . . H5 H 0.1591 0.3771 0.1444 0.040 Uiso 1 1 calc R . . C6 C 0.1033(3) 0.4107(6) 0.0980(5) 0.036(2) Uani 1 1 d . . . H6 H 0.0930 0.3764 0.0657 0.043 Uiso 1 1 calc R . . C7 C 0.2006(3) 0.4597(5) 0.2486(5) 0.028(2) Uani 1 1 d . . . C8 C 0.2122(3) 0.4885(5) 0.3130(4) 0.027(2) Uani 1 1 d . . . C9 C 0.1870(3) 0.4850(5) 0.3383(5) 0.029(2) Uani 1 1 d . . . H9 H 0.1635 0.4599 0.3146 0.034 Uiso 1 1 calc R . . C10 C 0.1951(3) 0.5162(6) 0.3951(5) 0.036(2) Uani 1 1 d . . . H10 H 0.1778 0.5115 0.4102 0.043 Uiso 1 1 calc R . . C11 C 0.2302(3) 0.5562(6) 0.4315(5) 0.033(2) Uani 1 1 d . . . C12 C 0.2571(3) 0.5579(5) 0.4093(5) 0.032(2) Uani 1 1 d . . . H12 H 0.2811 0.5814 0.4339 0.039 Uiso 1 1 calc R . . C13 C 0.2478(3) 0.5247(5) 0.3511(5) 0.032(2) Uani 1 1 d . . . H13 H 0.2657 0.5266 0.3370 0.038 Uiso 1 1 calc R . . C14 C 0.2302(3) 0.4321(5) 0.2380(5) 0.029(2) Uani 1 1 d . . . C15 C 0.2661(3) 0.4033(5) 0.2895(5) 0.030(2) Uani 1 1 d . . . H15 H 0.2706 0.4014 0.3322 0.036 Uiso 1 1 calc R . . C16 C 0.2943(3) 0.3780(5) 0.2787(5) 0.030(2) Uani 1 1 d . . . H16 H 0.3173 0.3583 0.3138 0.036 Uiso 1 1 calc R . . C17 C 0.2893(3) 0.3814(5) 0.2153(5) 0.030(2) Uani 1 1 d . . . C18 C 0.2538(3) 0.4086(6) 0.1636(5) 0.033(2) Uani 1 1 d . . . H18 H 0.2495 0.4103 0.1210 0.040 Uiso 1 1 calc R . . C19 C 0.2250(3) 0.4331(5) 0.1741(5) 0.030(2) Uani 1 1 d . . . H19 H 0.2015 0.4508 0.1384 0.036 Uiso 1 1 calc R . . C20 C 0.2537(3) 0.2703(5) 0.8529(5) 0.035(2) Uani 1 1 d . . . C21 C 0.2796(3) 0.2681(5) 0.8297(5) 0.032(2) Uani 1 1 d . . . H21 H 0.3044 0.2473 0.8553 0.039 Uiso 1 1 calc R . . C22 C 0.2683(3) 0.2974(6) 0.7677(5) 0.037(2) Uani 1 1 d . . . H22 H 0.2857 0.2961 0.7527 0.045 Uiso 1 1 calc R . . C23 C 0.2304(3) 0.3289(6) 0.7281(5) 0.034(2) Uani 1 1 d . . . C24 C 0.2051(3) 0.3286(6) 0.7533(5) 0.036(2) Uani 1 1 d . . . H24 H 0.1798 0.3476 0.7277 0.044 Uiso 1 1 calc R . . C25 C 0.2165(3) 0.3012(5) 0.8141(5) 0.033(2) Uani 1 1 d . . . H25 H 0.1993 0.3033 0.8297 0.039 Uiso 1 1 calc R . . C26 C 0.2177(3) 0.3589(6) 0.6642(5) 0.035(2) Uani 1 1 d . . . C27 C 0.2460(3) 0.3909(6) 0.6509(5) 0.039(3) Uani 1 1 d . . . C28 C 0.2818(3) 0.4204(6) 0.7020(5) 0.040(3) Uani 1 1 d . . . H28 H 0.2878 0.4180 0.7456 0.048 Uiso 1 1 calc R . . C29 C 0.3078(3) 0.4523(6) 0.6894(6) 0.045(3) Uani 1 1 d . . . H29 H 0.3313 0.4707 0.7245 0.054 Uiso 1 1 calc R . . C30 C 0.2994(4) 0.4577(7) 0.6240(6) 0.052(3) Uani 1 1 d . . . C31 C 0.2639(4) 0.4282(7) 0.5731(6) 0.056(4) Uani 1 1 d . . . H31 H 0.2580 0.4302 0.5295 0.067 Uiso 1 1 calc R . . C32 C 0.2380(3) 0.3968(7) 0.5857(6) 0.051(3) Uani 1 1 d . . . H32 H 0.2145 0.3787 0.5505 0.061 Uiso 1 1 calc R . . C33 C 0.1759(3) 0.3605(6) 0.6143(5) 0.034(2) Uani 1 1 d . . . C34 C 0.1575(3) 0.4165(6) 0.5708(5) 0.038(3) Uani 1 1 d . . . H34 H 0.1733 0.4520 0.5709 0.046 Uiso 1 1 calc R . . C35 C 0.1172(3) 0.4204(6) 0.5285(5) 0.041(3) Uani 1 1 d . . . H35 H 0.1060 0.4581 0.5003 0.049 Uiso 1 1 calc R . . C36 C 0.0924(3) 0.3672(6) 0.5276(5) 0.041(3) Uani 1 1 d . . . C37 C 0.1104(3) 0.3093(6) 0.5687(5) 0.037(3) Uani 1 1 d . . . H37 H 0.0949 0.2727 0.5674 0.045 Uiso 1 1 calc R . . C38 C 0.1505(3) 0.3075(6) 0.6101(5) 0.034(2) Uani 1 1 d . . . H38 H 0.1618 0.2691 0.6373 0.041 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0168(4) 0.0444(5) 0.0126(4) 0.0050(3) 0.0022(3) -0.0027(4) Mo2 0.0126(4) 0.0313(4) 0.0147(4) -0.0056(3) 0.0017(3) -0.0005(3) Mo3 0.0138(4) 0.0357(5) 0.0191(4) -0.0031(3) 0.0047(3) 0.0052(3) Mo4 0.0208(4) 0.0374(5) 0.0166(4) 0.0006(3) 0.0111(3) -0.0032(3) Mo5 0.0151(4) 0.0281(4) 0.0150(4) -0.0036(3) 0.0075(3) 0.0004(3) Mo6 0.0179(4) 0.0276(4) 0.0208(4) -0.0021(3) 0.0119(3) -0.0036(3) Mo7 0.0165(4) 0.0342(5) 0.0178(4) -0.0013(3) 0.0097(3) 0.0037(3) Mo8 0.0214(4) 0.0251(4) 0.0253(4) -0.0027(3) 0.0066(4) 0.0044(3) Mo9 0.0259(5) 0.0268(4) 0.0241(4) 0.0067(3) 0.0077(4) -0.0002(3) S1 0.0119(10) 0.0240(11) 0.0101(10) 0.0000(8) 0.0034(8) 0.0005(8) O1 0.023(4) 0.062(5) 0.016(3) 0.009(3) 0.000(3) -0.006(3) O2 0.014(3) 0.039(4) 0.019(3) -0.003(3) 0.002(3) 0.002(3) O3 0.019(3) 0.043(4) 0.025(3) -0.004(3) 0.008(3) 0.008(3) O4 0.018(3) 0.033(4) 0.011(3) -0.004(3) 0.002(3) 0.000(3) O5 0.012(3) 0.039(4) 0.012(3) -0.004(3) 0.004(2) 0.001(3) O6 0.016(3) 0.033(4) 0.014(3) 0.001(3) 0.002(3) 0.002(3) O7 0.018(3) 0.038(4) 0.016(3) 0.000(3) 0.009(3) -0.003(3) O8 0.016(3) 0.031(3) 0.013(3) 0.000(2) 0.006(3) 0.001(3) O9 0.015(3) 0.033(3) 0.014(3) -0.002(2) 0.008(3) -0.003(3) O10 0.014(3) 0.037(4) 0.018(3) -0.004(3) 0.006(3) 0.002(3) O11 0.017(3) 0.031(4) 0.017(3) -0.002(3) 0.002(3) 0.005(3) O12 0.018(3) 0.034(4) 0.017(3) 0.006(3) 0.001(3) 0.000(3) O13 0.013(3) 0.030(3) 0.013(3) 0.000(2) 0.006(3) 0.002(2) O14 0.009(3) 0.030(3) 0.010(3) 0.004(2) 0.003(2) 0.001(2) O15 0.015(3) 0.025(3) 0.016(3) -0.001(2) 0.009(3) 0.000(2) O16 0.017(3) 0.028(3) 0.016(3) 0.002(3) 0.005(3) 0.002(3) O17 0.022(4) 0.054(5) 0.018(3) 0.003(3) 0.010(3) -0.002(3) O18 0.013(3) 0.040(4) 0.008(3) -0.001(3) 0.003(2) 0.001(3) O19 0.017(3) 0.037(4) 0.021(3) -0.006(3) 0.003(3) 0.005(3) O20 0.017(3) 0.024(3) 0.014(3) -0.001(2) 0.007(3) 0.000(2) O21 0.020(3) 0.036(4) 0.022(3) 0.001(3) 0.008(3) -0.004(3) O22 0.012(3) 0.035(4) 0.012(3) -0.001(2) 0.005(2) 0.000(3) O23 0.018(3) 0.052(4) 0.020(3) -0.004(3) 0.010(3) 0.005(3) O24 0.019(3) 0.030(3) 0.018(3) -0.001(3) 0.006(3) 0.004(3) O25 0.026(4) 0.041(4) 0.034(4) -0.009(3) 0.006(3) 0.007(3) O26 0.021(3) 0.026(3) 0.022(3) 0.003(3) 0.000(3) 0.003(3) O27 0.039(4) 0.037(4) 0.029(4) 0.010(3) 0.008(3) -0.006(3) O28 0.017(3) 0.034(4) 0.018(3) 0.007(3) 0.005(3) -0.001(3) O29 0.015(3) 0.033(4) 0.014(3) 0.000(2) 0.008(3) 0.001(3) O30 0.015(3) 0.038(4) 0.013(3) 0.000(3) 0.005(3) 0.005(3) O31 0.020(3) 0.035(4) 0.022(3) -0.003(3) 0.005(3) 0.006(3) N1 0.022(5) 0.080(7) 0.029(5) -0.017(5) 0.004(4) 0.010(5) N2 0.027(5) 0.069(7) 0.031(5) -0.021(5) 0.012(4) -0.005(4) N3 0.027(5) 0.052(6) 0.032(5) -0.006(4) 0.017(4) 0.010(4) N4 0.024(5) 0.056(6) 0.017(4) 0.004(4) -0.003(4) 0.002(4) N5 0.048(7) 0.141(13) 0.051(7) 0.005(8) 0.020(6) -0.044(8) N6 0.021(5) 0.067(7) 0.056(6) 0.034(6) 0.004(5) 0.003(5) C1 0.024(5) 0.065(7) 0.014(4) -0.004(5) 0.009(4) 0.005(5) C2 0.026(5) 0.058(7) 0.022(5) -0.002(5) 0.015(4) 0.013(5) C3 0.022(5) 0.043(6) 0.018(4) -0.011(4) 0.007(4) 0.003(4) C4 0.020(5) 0.043(6) 0.021(5) -0.010(4) 0.011(4) -0.004(4) C5 0.024(5) 0.052(7) 0.025(5) -0.011(5) 0.013(4) 0.004(5) C6 0.028(6) 0.059(7) 0.020(5) -0.016(5) 0.012(4) -0.004(5) C7 0.023(5) 0.034(5) 0.030(5) -0.005(4) 0.015(4) 0.001(4) C8 0.015(5) 0.041(6) 0.017(4) -0.002(4) 0.003(4) 0.009(4) C9 0.016(5) 0.045(6) 0.020(5) -0.009(4) 0.007(4) 0.002(4) C10 0.019(5) 0.055(7) 0.025(5) -0.007(5) 0.007(4) 0.007(5) C11 0.021(5) 0.048(6) 0.017(5) -0.010(4) 0.001(4) 0.006(4) C12 0.019(5) 0.039(6) 0.025(5) -0.008(4) 0.002(4) 0.002(4) C13 0.018(5) 0.045(6) 0.023(5) -0.002(4) 0.005(4) 0.011(4) C14 0.019(5) 0.038(6) 0.025(5) -0.009(4) 0.010(4) 0.001(4) C15 0.023(5) 0.042(6) 0.021(5) -0.004(4) 0.009(4) 0.002(4) C16 0.019(5) 0.039(6) 0.021(5) 0.002(4) 0.004(4) 0.011(4) C17 0.023(5) 0.037(6) 0.027(5) -0.008(4) 0.011(4) 0.000(4) C18 0.028(5) 0.046(6) 0.024(5) -0.002(4) 0.013(4) 0.006(5) C19 0.018(5) 0.044(6) 0.021(5) 0.000(4) 0.007(4) 0.009(4) C20 0.026(5) 0.031(6) 0.032(6) -0.003(4) 0.005(5) -0.005(4) C21 0.017(5) 0.038(6) 0.027(5) 0.009(4) 0.001(4) 0.002(4) C22 0.020(5) 0.042(6) 0.040(6) 0.003(5) 0.009(5) -0.001(4) C23 0.023(5) 0.043(6) 0.024(5) 0.004(4) 0.003(4) -0.002(4) C24 0.021(5) 0.041(6) 0.031(6) 0.004(5) 0.003(4) 0.005(4) C25 0.021(5) 0.039(6) 0.026(5) 0.000(4) 0.004(4) -0.004(4) C26 0.026(5) 0.037(6) 0.034(6) 0.004(5) 0.010(5) -0.002(4) C27 0.028(6) 0.045(6) 0.031(6) 0.007(5) 0.007(5) -0.003(5) C28 0.024(5) 0.048(7) 0.031(6) 0.006(5) 0.003(5) -0.002(5) C29 0.026(6) 0.050(7) 0.043(7) 0.005(5) 0.006(5) -0.011(5) C30 0.035(7) 0.064(8) 0.044(7) 0.009(6) 0.013(6) -0.013(6) C31 0.047(8) 0.076(9) 0.036(6) 0.005(6) 0.016(6) -0.022(7) C32 0.024(6) 0.074(9) 0.039(6) 0.007(6) 0.006(5) -0.015(6) C33 0.028(5) 0.040(6) 0.022(5) 0.006(4) 0.006(4) -0.002(4) C34 0.029(6) 0.045(6) 0.028(5) 0.003(5) 0.006(5) -0.011(5) C35 0.032(6) 0.039(6) 0.033(6) 0.012(5) 0.004(5) -0.002(5) C36 0.029(6) 0.053(7) 0.033(6) 0.016(5) 0.011(5) 0.003(5) C37 0.024(5) 0.043(6) 0.030(5) 0.006(5) 0.004(5) -0.008(5) C38 0.027(5) 0.038(6) 0.022(5) 0.011(4) 0.002(4) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.690(6) . ? Mo1 O12 1.836(6) . ? Mo1 O6 1.849(6) . ? Mo1 O4 1.980(7) . ? Mo1 O7 1.986(6) . ? Mo1 O13 2.511(6) . ? Mo2 O2 1.690(6) . ? Mo2 O8 1.809(6) . ? Mo2 O4 1.859(6) . ? Mo2 O5 1.956(6) . ? Mo2 O9 1.993(6) . ? Mo2 O13 2.480(6) . ? Mo3 O3 1.697(6) . ? Mo3 O10 1.812(6) . ? Mo3 O11 1.873(6) . ? Mo3 O5 1.902(6) . ? Mo3 O6 2.026(6) . ? Mo3 O13 2.445(6) . ? Mo4 O17 1.690(6) . ? Mo4 O7 1.853(6) . ? Mo4 O28 1.854(7) . ? Mo4 O18 1.923(7) . ? Mo4 O30 1.981(6) 2_556 ? Mo4 O14 2.459(6) . ? Mo5 O19 1.695(7) . ? Mo5 O29 1.802(6) . ? Mo5 O20 1.880(6) . ? Mo5 O18 1.907(6) . ? Mo5 O8 2.066(6) . ? Mo5 O14 2.443(6) . ? Mo6 O21 1.671(7) . ? Mo6 O9 1.834(6) . ? Mo6 O22 1.873(6) . ? Mo6 O20 1.904(6) . ? Mo6 O29 2.023(6) 2_556 ? Mo6 O15 2.483(6) . ? Mo7 O23 1.683(6) . ? Mo7 O30 1.826(6) . ? Mo7 O24 1.841(7) . ? Mo7 O22 1.933(6) . ? Mo7 O10 2.083(6) . ? Mo7 O15 2.481(6) . ? Mo8 O25 1.685(7) . ? Mo8 O31 1.871(6) . ? Mo8 O26 1.883(7) . ? Mo8 O24 1.937(7) . ? Mo8 O11 1.985(6) . ? Mo8 O16 2.476(6) . ? Mo9 O27 1.683(7) . ? Mo9 O31 1.893(6) 2_556 ? Mo9 O26 1.899(7) . ? Mo9 O28 1.942(7) . ? Mo9 O12 1.972(6) . ? Mo9 O16 2.480(6) . ? S1 O16 1.454(7) . ? S1 O15 1.461(6) . ? S1 O14 1.466(6) . ? S1 O13 1.492(6) . ? O29 Mo6 2.023(6) 2_556 ? O30 Mo4 1.981(6) 2_556 ? O31 Mo9 1.893(6) 2_556 ? N1 C1 1.354(13) . ? N1 H1A 0.8600 . ? N1 H1B 0.8600 . ? N2 C11 1.348(13) . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? N3 C17 1.344(13) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? N4 C20 1.341(14) . ? N4 H4A 0.8600 . ? N4 H4B 0.8600 . ? N5 C30 1.352(16) . ? N5 H5A 0.8600 . ? N5 H5B 0.8600 . ? N6 C36 1.354(14) . ? N6 H6A 0.8600 . ? N6 H6B 0.8600 . ? C1 C2 1.378(15) . ? C1 C6 1.397(15) . ? C2 C3 1.370(13) . ? C2 H2 0.9300 . ? C3 C4 1.413(14) . ? C3 H3 0.9300 . ? C4 C5 1.407(14) . ? C4 C7 1.434(13) . ? C5 C6 1.357(14) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C14 1.425(13) . ? C7 C8 1.451(13) . ? C8 C13 1.397(14) . ? C8 C9 1.410(13) . ? C9 C10 1.348(13) . ? C9 H9 0.9300 . ? C10 C11 1.417(15) . ? C10 H10 0.9300 . ? C11 C12 1.414(15) . ? C12 C13 1.381(14) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.409(13) . ? C14 C19 1.413(13) . ? C15 C16 1.363(14) . ? C15 H15 0.9300 . ? C16 C17 1.405(14) . ? C16 H16 0.9300 . ? C17 C18 1.390(14) . ? C18 C19 1.373(14) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? C20 C25 1.395(14) . ? C20 C21 1.395(16) . ? C21 C22 1.407(15) . ? C21 H21 0.9300 . ? C22 C23 1.418(14) . ? C22 H22 0.9300 . ? C23 C24 1.412(16) . ? C23 C26 1.438(14) . ? C24 C25 1.367(15) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C33 1.438(14) . ? C26 C27 1.452(15) . ? C27 C28 1.409(15) . ? C27 C32 1.408(17) . ? C28 C29 1.362(16) . ? C28 H28 0.9300 . ? C29 C30 1.404(17) . ? C29 H29 0.9300 . ? C30 C31 1.400(17) . ? C31 C32 1.356(17) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C38 1.404(15) . ? C33 C34 1.409(15) . ? C34 C35 1.363(15) . ? C34 H34 0.9300 . ? C35 C36 1.418(16) . ? C35 H35 0.9300 . ? C36 C37 1.409(15) . ? C37 C38 1.354(14) . ? C37 H37 0.9300 . ? C38 H38 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O12 104.6(3) . . ? O1 Mo1 O6 103.8(3) . . ? O12 Mo1 O6 94.0(3) . . ? O1 Mo1 O4 101.0(3) . . ? O12 Mo1 O4 153.6(3) . . ? O6 Mo1 O4 86.3(3) . . ? O1 Mo1 O7 102.3(3) . . ? O12 Mo1 O7 85.8(3) . . ? O6 Mo1 O7 153.1(3) . . ? O4 Mo1 O7 82.3(3) . . ? O1 Mo1 O13 173.3(3) . . ? O12 Mo1 O13 81.8(2) . . ? O6 Mo1 O13 73.6(2) . . ? O4 Mo1 O13 72.9(2) . . ? O7 Mo1 O13 79.8(2) . . ? O2 Mo2 O8 105.7(3) . . ? O2 Mo2 O4 103.6(3) . . ? O8 Mo2 O4 96.0(3) . . ? O2 Mo2 O5 100.0(3) . . ? O8 Mo2 O5 152.9(3) . . ? O4 Mo2 O5 86.0(3) . . ? O2 Mo2 O9 100.2(3) . . ? O8 Mo2 O9 85.1(2) . . ? O4 Mo2 O9 154.9(3) . . ? O5 Mo2 O9 82.1(2) . . ? O2 Mo2 O13 170.9(3) . . ? O8 Mo2 O13 83.4(2) . . ? O4 Mo2 O13 75.6(2) . . ? O5 Mo2 O13 70.9(2) . . ? O9 Mo2 O13 79.7(2) . . ? O3 Mo3 O10 103.2(3) . . ? O3 Mo3 O11 103.5(3) . . ? O10 Mo3 O11 90.4(3) . . ? O3 Mo3 O5 101.8(3) . . ? O10 Mo3 O5 91.9(3) . . ? O11 Mo3 O5 153.4(3) . . ? O3 Mo3 O6 99.8(3) . . ? O10 Mo3 O6 157.0(3) . . ? O11 Mo3 O6 85.0(3) . . ? O5 Mo3 O6 82.5(3) . . ? O3 Mo3 O13 170.7(3) . . ? O10 Mo3 O13 84.6(2) . . ? O11 Mo3 O13 81.3(2) . . ? O5 Mo3 O13 72.5(2) . . ? O6 Mo3 O13 72.5(2) . . ? O17 Mo4 O7 100.9(3) . . ? O17 Mo4 O28 105.2(3) . . ? O7 Mo4 O28 90.1(3) . . ? O17 Mo4 O18 101.1(3) . . ? O7 Mo4 O18 90.9(3) . . ? O28 Mo4 O18 153.0(3) . . ? O17 Mo4 O30 97.0(3) . 2_556 ? O7 Mo4 O30 162.0(3) . 2_556 ? O28 Mo4 O30 85.7(3) . 2_556 ? O18 Mo4 O30 85.1(3) . 2_556 ? O17 Mo4 O14 170.8(3) . . ? O7 Mo4 O14 83.8(2) . . ? O28 Mo4 O14 82.5(2) . . ? O18 Mo4 O14 70.8(2) . . ? O30 Mo4 O14 78.3(2) 2_556 . ? O19 Mo5 O29 101.2(3) . . ? O19 Mo5 O20 104.0(3) . . ? O29 Mo5 O20 93.0(3) . . ? O19 Mo5 O18 100.4(3) . . ? O29 Mo5 O18 94.5(3) . . ? O20 Mo5 O18 152.6(3) . . ? O19 Mo5 O8 96.0(3) . . ? O29 Mo5 O8 162.8(3) . . ? O20 Mo5 O8 81.3(2) . . ? O18 Mo5 O8 83.9(2) . . ? O19 Mo5 O14 170.6(3) . . ? O29 Mo5 O14 84.3(2) . . ? O20 Mo5 O14 83.2(2) . . ? O18 Mo5 O14 71.4(2) . . ? O8 Mo5 O14 78.9(2) . . ? O21 Mo6 O9 102.1(3) . . ? O21 Mo6 O22 103.3(3) . . ? O9 Mo6 O22 94.6(3) . . ? O21 Mo6 O20 103.3(3) . . ? O9 Mo6 O20 88.7(2) . . ? O22 Mo6 O20 151.9(3) . . ? O21 Mo6 O29 96.5(3) . 2_556 ? O9 Mo6 O29 161.0(3) . 2_556 ? O22 Mo6 O29 85.0(2) . 2_556 ? O20 Mo6 O29 83.1(2) . 2_556 ? O21 Mo6 O15 172.9(3) . . ? O9 Mo6 O15 83.9(2) . . ? O22 Mo6 O15 72.1(2) . . ? O20 Mo6 O15 80.5(2) . . ? O29 Mo6 O15 77.9(2) 2_556 . ? O23 Mo7 O30 102.5(3) . . ? O23 Mo7 O24 101.9(3) . . ? O30 Mo7 O24 95.7(3) . . ? O23 Mo7 O22 103.4(3) . . ? O30 Mo7 O22 91.7(3) . . ? O24 Mo7 O22 151.4(3) . . ? O23 Mo7 O10 94.6(3) . . ? O30 Mo7 O10 162.8(3) . . ? O24 Mo7 O10 82.5(3) . . ? O22 Mo7 O10 82.4(2) . . ? O23 Mo7 O15 171.2(3) . . ? O30 Mo7 O15 84.9(2) . . ? O24 Mo7 O15 81.8(2) . . ? O22 Mo7 O15 71.3(2) . . ? O10 Mo7 O15 77.9(2) . . ? O25 Mo8 O31 100.4(3) . . ? O25 Mo8 O26 102.7(3) . . ? O31 Mo8 O26 92.3(3) . . ? O25 Mo8 O24 104.7(3) . . ? O31 Mo8 O24 87.0(3) . . ? O26 Mo8 O24 152.3(3) . . ? O25 Mo8 O11 97.1(3) . . ? O31 Mo8 O11 161.5(3) . . ? O26 Mo8 O11 89.6(3) . . ? O24 Mo8 O11 82.9(3) . . ? O25 Mo8 O16 173.1(3) . . ? O31 Mo8 O16 83.4(2) . . ? O26 Mo8 O16 71.3(2) . . ? O24 Mo8 O16 81.1(2) . . ? O11 Mo8 O16 79.8(2) . . ? O27 Mo9 O31 100.5(3) . 2_556 ? O27 Mo9 O26 102.3(3) . . ? O31 Mo9 O26 90.7(3) 2_556 . ? O27 Mo9 O28 104.4(3) . . ? O31 Mo9 O28 89.7(3) 2_556 . ? O26 Mo9 O28 152.7(3) . . ? O27 Mo9 O12 97.4(3) . . ? O31 Mo9 O12 161.7(3) 2_556 . ? O26 Mo9 O12 88.9(3) . . ? O28 Mo9 O12 82.4(3) . . ? O27 Mo9 O16 172.9(3) . . ? O31 Mo9 O16 82.4(2) 2_556 . ? O26 Mo9 O16 71.0(2) . . ? O28 Mo9 O16 82.0(2) . . ? O12 Mo9 O16 80.2(2) . . ? O16 S1 O15 110.5(4) . . ? O16 S1 O14 110.7(4) . . ? O15 S1 O14 110.7(3) . . ? O16 S1 O13 108.6(3) . . ? O15 S1 O13 108.5(3) . . ? O14 S1 O13 107.7(3) . . ? Mo2 O4 Mo1 125.3(3) . . ? Mo3 O5 Mo2 127.4(3) . . ? Mo1 O6 Mo3 125.8(3) . . ? Mo4 O7 Mo1 147.3(4) . . ? Mo2 O8 Mo5 154.6(3) . . ? Mo6 O9 Mo2 149.2(3) . . ? Mo3 O10 Mo7 148.6(4) . . ? Mo3 O11 Mo8 149.9(4) . . ? Mo1 O12 Mo9 156.5(4) . . ? S1 O13 Mo3 125.5(3) . . ? S1 O13 Mo2 127.5(3) . . ? Mo3 O13 Mo2 89.20(19) . . ? S1 O13 Mo1 127.3(3) . . ? Mo3 O13 Mo1 88.22(19) . . ? Mo2 O13 Mo1 86.17(18) . . ? S1 O14 Mo5 129.5(3) . . ? S1 O14 Mo4 126.7(3) . . ? Mo5 O14 Mo4 89.35(19) . . ? S1 O15 Mo7 129.7(3) . . ? S1 O15 Mo6 126.3(3) . . ? Mo7 O15 Mo6 87.57(18) . . ? S1 O16 Mo8 128.4(4) . . ? S1 O16 Mo9 128.5(3) . . ? Mo8 O16 Mo9 87.5(2) . . ? Mo5 O18 Mo4 128.2(3) . . ? Mo5 O20 Mo6 154.3(3) . . ? Mo6 O22 Mo7 128.9(3) . . ? Mo7 O24 Mo8 159.6(4) . . ? Mo8 O26 Mo9 130.0(4) . . ? Mo4 O28 Mo9 152.1(4) . . ? Mo5 O29 Mo6 164.7(3) . 2_556 ? Mo7 O30 Mo4 160.8(4) . 2_556 ? Mo8 O31 Mo9 166.9(4) . 2_556 ? C1 N1 H1A 120.0 . . ? C1 N1 H1B 120.0 . . ? H1A N1 H1B 120.0 . . ? C11 N2 H2A 120.0 . . ? C11 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C17 N3 H3A 120.0 . . ? C17 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C20 N4 H4A 120.0 . . ? C20 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C30 N5 H5A 120.0 . . ? C30 N5 H5B 120.0 . . ? H5A N5 H5B 120.0 . . ? C36 N6 H6A 120.0 . . ? C36 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? N1 C1 C2 120.7(10) . . ? N1 C1 C6 120.4(10) . . ? C2 C1 C6 118.9(9) . . ? C1 C2 C3 120.2(10) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C2 C3 C4 122.1(9) . . ? C2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? C5 C4 C3 116.2(9) . . ? C5 C4 C7 122.3(9) . . ? C3 C4 C7 121.5(8) . . ? C6 C5 C4 121.5(10) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C1 121.1(9) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? C14 C7 C4 121.2(9) . . ? C14 C7 C8 119.9(8) . . ? C4 C7 C8 118.8(8) . . ? C13 C8 C9 116.6(9) . . ? C13 C8 C7 121.5(9) . . ? C9 C8 C7 121.8(9) . . ? C10 C9 C8 123.4(9) . . ? C10 C9 H9 118.3 . . ? C8 C9 H9 118.3 . . ? C9 C10 C11 119.7(10) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? N2 C11 C12 121.0(10) . . ? N2 C11 C10 120.7(10) . . ? C12 C11 C10 118.3(9) . . ? C13 C12 C11 120.2(9) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C8 121.7(10) . . ? C12 C13 H13 119.2 . . ? C8 C13 H13 119.2 . . ? C15 C14 C19 116.2(9) . . ? C15 C14 C7 122.8(9) . . ? C19 C14 C7 121.0(9) . . ? C16 C15 C14 122.1(9) . . ? C16 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C15 C16 C17 121.0(9) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? N3 C17 C18 121.2(9) . . ? N3 C17 C16 121.1(9) . . ? C18 C17 C16 117.7(9) . . ? C19 C18 C17 121.4(9) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C18 C19 C14 121.6(9) . . ? C18 C19 H19 119.2 . . ? C14 C19 H19 119.2 . . ? N4 C20 C25 120.4(11) . . ? N4 C20 C21 120.0(10) . . ? C25 C20 C21 119.6(10) . . ? C20 C21 C22 120.2(9) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C21 C22 C23 120.5(10) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C24 C23 C22 117.0(9) . . ? C24 C23 C26 120.8(9) . . ? C22 C23 C26 122.1(10) . . ? C25 C24 C23 122.3(10) . . ? C25 C24 H24 118.8 . . ? C23 C24 H24 118.8 . . ? C24 C25 C20 120.4(10) . . ? C24 C25 H25 119.8 . . ? C20 C25 H25 119.8 . . ? C33 C26 C23 118.9(9) . . ? C33 C26 C27 119.8(9) . . ? C23 C26 C27 121.2(9) . . ? C28 C27 C32 116.6(10) . . ? C28 C27 C26 121.9(10) . . ? C32 C27 C26 121.4(10) . . ? C29 C28 C27 122.1(11) . . ? C29 C28 H28 118.9 . . ? C27 C28 H28 118.9 . . ? C28 C29 C30 120.5(11) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? N5 C30 C29 121.5(11) . . ? N5 C30 C31 120.8(12) . . ? C29 C30 C31 117.7(11) . . ? C32 C31 C30 121.6(12) . . ? C32 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? C31 C32 C27 121.5(11) . . ? C31 C32 H32 119.3 . . ? C27 C32 H32 119.3 . . ? C38 C33 C34 116.2(9) . . ? C38 C33 C26 120.8(9) . . ? C34 C33 C26 122.8(10) . . ? C35 C34 C33 122.1(10) . . ? C35 C34 H34 119.0 . . ? C33 C34 H34 119.0 . . ? C34 C35 C36 120.1(10) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? N6 C36 C37 120.8(10) . . ? N6 C36 C35 120.6(10) . . ? C37 C36 C35 118.6(10) . . ? C38 C37 C36 119.4(10) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C37 C38 C33 123.6(10) . . ? C37 C38 H38 118.2 . . ? C33 C38 H38 118.2 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.956 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.249 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 619195' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C101.50 H131.50 Mo8 N20.50 O34.50' _chemical_formula_weight 2958.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Mo Mo -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 16.0479(16) _cell_length_b 16.3393(16) _cell_length_c 26.093(3) _cell_angle_alpha 84.935(2) _cell_angle_beta 89.470(2) _cell_angle_gamma 63.896(2) _cell_volume 6116.6(10) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 6 _cell_measurement_theta_max 12 _exptl_crystal_description block _exptl_crystal_colour black-purple _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.606 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 0.875 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.841 _exptl_absorpt_correction_T_max 0.880 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31929 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.0892 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 0.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 21116 _reflns_number_gt 12929 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SMART (Siemens, 1996)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990) ; _refine_special_details ; The crystal contains large amounts of solvent and while much of the solvent (dmf) could be assigned, a significant proportion of the solvent could not be satisfactorily modelled. Using the SQUEEZE routine within platon a volume of 1011F^-3^ was identified within the unit cell that contained an estimated 210 electrons. This is consistent with approximately 5 dmf molecules per unit cell or 2.5 molecules of dmf per formula unit. This gives a total of 8.5 dmf molecules in each formula unit. The reflection data was modified with the contribution of the disordered solvent eliminated from the data. 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^)+(0.1001P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 21116 _refine_ls_number_parameters 1226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1009 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1931 _refine_ls_wR_factor_gt 0.1777 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.63852(5) 0.46309(4) 0.19043(2) 0.02986(17) Uani 1 1 d . . . Mo2 Mo 0.51085(4) 0.35093(4) 0.19306(2) 0.02726(17) Uani 1 1 d . . . Mo3 Mo 0.56625(4) 0.52614(4) 0.30417(2) 0.02355(16) Uani 1 1 d . . . Mo4 Mo 0.40030(4) 0.58763(4) 0.20160(2) 0.02421(16) Uani 1 1 d . . . Mo5 Mo 0.27515(4) 0.47713(4) 0.20431(2) 0.02934(17) Uani 1 1 d . . . Mo6 Mo 0.44192(4) 0.41519(4) 0.30560(2) 0.02164(15) Uani 1 1 d . . . Mo7 Mo 0.33087(4) 0.65397(4) 0.31309(2) 0.02224(15) Uani 1 1 d . . . Mo8 Mo 0.20245(4) 0.54428(4) 0.31747(2) 0.02495(16) Uani 1 1 d . . . O1 O 0.6914(4) 0.4981(4) 0.1430(2) 0.0460(14) Uani 1 1 d . . . O2 O 0.7262(3) 0.3682(3) 0.22164(19) 0.0419(14) Uani 1 1 d . . . O3 O 0.6197(3) 0.5468(3) 0.24148(17) 0.0290(11) Uani 1 1 d . . . O4 O 0.4978(3) 0.5803(3) 0.16656(17) 0.0317(12) Uani 1 1 d . . . O5 O 0.5801(3) 0.4023(3) 0.15406(17) 0.0326(12) Uani 1 1 d . . . O6 O 0.4718(4) 0.3092(3) 0.14533(18) 0.0373(13) Uani 1 1 d . . . O7 O 0.5976(3) 0.2553(3) 0.22426(18) 0.0354(12) Uani 1 1 d . . . O8 O 0.5149(3) 0.4551(3) 0.24593(16) 0.0235(10) Uani 1 1 d . . . O9 O 0.6527(3) 0.4251(3) 0.33080(18) 0.0310(12) Uani 1 1 d . . . O10 O 0.5691(3) 0.6089(3) 0.33927(17) 0.0293(11) Uani 1 1 d . . . O11 O 0.4300(3) 0.6341(3) 0.26132(16) 0.0252(11) Uani 1 1 d . . . O12 O 0.3091(3) 0.6835(3) 0.17483(18) 0.0342(12) Uani 1 1 d . . . O13 O 0.3822(3) 0.4918(3) 0.17132(16) 0.0275(11) Uani 1 1 d . . . O14 O 0.2722(4) 0.3935(4) 0.17034(19) 0.0449(14) Uani 1 1 d . . . O15 O 0.4132(3) 0.3685(3) 0.24513(17) 0.0282(11) Uani 1 1 d . . . O16 O 0.5345(3) 0.3208(3) 0.33264(17) 0.0306(12) Uani 1 1 d . . . O17 O 0.4583(3) 0.5121(3) 0.33615(16) 0.0237(10) Uani 1 1 d . . . O18 O 0.3691(3) 0.6975(3) 0.35912(17) 0.0285(11) Uani 1 1 d . . . O19 O 0.2444(3) 0.7484(3) 0.28038(18) 0.0295(11) Uani 1 1 d . . . O20 O 0.3260(3) 0.5494(3) 0.26068(15) 0.0227(10) Uani 1 1 d . . . O21 O 0.1896(3) 0.5770(3) 0.17636(18) 0.0389(13) Uani 1 1 d . . . O22 O 0.2199(3) 0.4606(3) 0.26613(17) 0.0284(11) Uani 1 1 d . . . O23 O 0.3456(3) 0.4240(3) 0.34172(16) 0.0283(11) Uani 1 1 d . . . O24 O 0.2637(3) 0.6028(3) 0.35356(16) 0.0249(10) Uani 1 1 d . . . O25 O 0.1132(3) 0.6393(3) 0.28835(19) 0.0350(12) Uani 1 1 d . . . O26 O 0.1531(3) 0.5074(3) 0.36736(17) 0.0323(12) Uani 1 1 d . . . O27 O 0.5793(3) 0.5663(3) 0.46650(18) 0.0326(12) Uiso 1 1 d . . . O28 O -0.0312(4) 0.1740(4) 0.2413(2) 0.0446(14) Uiso 1 1 d . . . O29 O 0.1781(3) 0.0408(3) 0.74581(19) 0.0371(12) Uiso 1 1 d . . . O30 O 0.3154(4) 0.5269(5) 0.9892(3) 0.0700(19) Uiso 1 1 d . . . O31 O 0.7198(3) 0.9573(3) 0.75687(19) 0.0368(12) Uiso 1 1 d . . . O32 O 0.3722(4) 0.1713(4) 0.74271(19) 0.0480(15) Uani 1 1 d . . . N1 N 0.8096(5) 1.1917(4) 0.1778(3) 0.0486(18) Uani 1 1 d . . . H1A H 0.8497 1.1776 0.2037 0.058 Uiso 1 1 calc R . . H1B H 0.7546 1.2387 0.1785 0.058 Uiso 1 1 calc R . . N2 N 1.1615(6) 0.6041(6) 0.0598(3) 0.076(3) Uiso 1 1 d . . . H2A H 1.1651 0.5776 0.0911 0.092 Uiso 1 1 calc R . . H2B H 1.2013 0.5748 0.0368 0.092 Uiso 1 1 calc R . . N3 N 0.7450(4) 1.1075(4) -0.1880(2) 0.0332(15) Uani 1 1 d . . . H3A H 0.7347 1.0717 -0.2077 0.040 Uiso 1 1 calc R . . H3B H 0.7315 1.1643 -0.1996 0.040 Uiso 1 1 calc R . . N4 N 0.7759(4) 1.0736(4) 0.6850(2) 0.0294(14) Uani 1 1 d . . . H4A H 0.7669 1.1273 0.6944 0.035 Uiso 1 1 calc R . . H4B H 0.7680 1.0340 0.7072 0.035 Uiso 1 1 calc R . . N5 N 1.1373(4) 0.6011(4) 0.4695(2) 0.0324(14) Uani 1 1 d . . . H5A H 1.1738 0.5682 0.4960 0.039 Uiso 1 1 calc R . . H5B H 1.1382 0.5758 0.4410 0.039 Uiso 1 1 calc R . . N6 N 0.8094(4) 1.2374(4) 0.3138(2) 0.0340(15) Uani 1 1 d . . . H6A H 0.7573 1.2882 0.3124 0.041 Uiso 1 1 calc R . . H6B H 0.8483 1.2276 0.2885 0.041 Uiso 1 1 calc R . . N7 N 0.3335(4) -0.1043(4) 0.6883(2) 0.0303(14) Uani 1 1 d . . . H7A H 0.3702 -0.1614 0.6996 0.036 Uiso 1 1 calc R . . H7B H 0.2897 -0.0692 0.7079 0.036 Uiso 1 1 calc R . . N8 N 0.4859(4) -0.1865(4) 0.3256(2) 0.0377(16) Uani 1 1 d . . . H8A H 0.4789 -0.2371 0.3268 0.045 Uiso 1 1 calc R . . H8B H 0.5118 -0.1712 0.2990 0.045 Uiso 1 1 calc R . . N9 N 0.3095(4) 0.4067(4) 0.4557(2) 0.0276(13) Uani 1 1 d . . . H9A H 0.3262 0.4307 0.4802 0.033 Uiso 1 1 calc R . . H9B H 0.2867 0.4392 0.4260 0.033 Uiso 1 1 calc R . . N10 N 0.5458(4) -0.2539(4) 0.1850(2) 0.0362(15) Uani 1 1 d . . . H10A H 0.5372 -0.3037 0.1881 0.043 Uiso 1 1 calc R . . H10B H 0.5807 -0.2458 0.2079 0.043 Uiso 1 1 calc R . . N11 N 0.3377(4) -0.0692(4) -0.1807(2) 0.0289(14) Uani 1 1 d . . . H11A H 0.3743 -0.1237 -0.1902 0.035 Uiso 1 1 calc R . . H11B H 0.2950 -0.0284 -0.2024 0.035 Uiso 1 1 calc R . . N12 N 0.3104(4) 0.3780(4) 0.0556(2) 0.0361(15) Uani 1 1 d . . . H12A H 0.2960 0.3966 0.0865 0.043 Uiso 1 1 calc R . . H12B H 0.3165 0.4146 0.0306 0.043 Uiso 1 1 calc R . . N13 N 0.4278(4) 0.6257(4) 0.4899(2) 0.0328(14) Uiso 1 1 d . . . N14 N 0.0316(5) 0.2493(5) 0.1892(3) 0.0501(18) Uiso 1 1 d . . . N15 N 0.0206(4) 0.1205(4) 0.7563(2) 0.0300(14) Uiso 1 1 d . . . N16 N 0.4037(5) 0.6067(5) 0.9981(3) 0.057(2) Uiso 1 1 d . . . N17 N 0.6277(5) 0.8834(5) 0.7512(3) 0.0451(17) Uiso 1 1 d . . . N18 N 0.2396(5) 0.2496(5) 0.6933(3) 0.0470(18) Uiso 1 1 d . . . C1 C 0.8966(4) 0.9706(4) 0.0136(2) 0.0211(14) Uani 1 1 d . . . C2 C 0.8759(4) 1.0293(4) 0.0543(2) 0.0213(15) Uani 1 1 d . . . C3 C 0.7886(5) 1.1103(4) 0.0553(3) 0.0247(15) Uani 1 1 d . . . H3 H 0.7447 1.1270 0.0276 0.030 Uiso 1 1 calc R . . C4 C 0.7685(5) 1.1630(5) 0.0957(3) 0.0264(16) Uani 1 1 d . . . H4 H 0.7103 1.2155 0.0956 0.032 Uiso 1 1 calc R . . C5 C 0.8320(5) 1.1416(5) 0.1375(3) 0.0346(18) Uani 1 1 d . . . C6 C 0.9198(5) 1.0659(5) 0.1359(3) 0.0323(18) Uani 1 1 d . . . H6 H 0.9654 1.0531 0.1623 0.039 Uiso 1 1 calc R . . C7 C 0.9397(5) 1.0109(5) 0.0964(2) 0.0237(15) Uani 1 1 d . . . H7 H 0.9980 0.9585 0.0971 0.028 Uiso 1 1 calc R . . C8 C 0.9598(4) 0.8728(4) 0.0236(2) 0.0232(15) Uani 1 1 d . . . C9 C 0.9652(5) 0.8270(5) 0.0729(3) 0.0321(18) Uani 1 1 d . . . H9 H 0.9235 0.8582 0.0985 0.039 Uiso 1 1 calc R . . C10 C 1.0309(5) 0.7369(5) 0.0844(3) 0.044(2) Uani 1 1 d . . . H10 H 1.0332 0.7062 0.1174 0.052 Uiso 1 1 calc R . . C11 C 1.0939(6) 0.6912(5) 0.0470(3) 0.052(2) Uani 1 1 d . . . C12 C 1.0856(5) 0.7359(5) -0.0030(3) 0.040(2) Uani 1 1 d . . . H12 H 1.1254 0.7041 -0.0291 0.048 Uiso 1 1 calc R . . C13 C 1.0220(4) 0.8228(4) -0.0138(2) 0.0245(16) Uani 1 1 d . . . H13 H 1.0183 0.8519 -0.0474 0.029 Uiso 1 1 calc R . . C14 C 0.8566(4) 1.0058(4) -0.0383(2) 0.0204(15) Uani 1 1 d . . . C15 C 0.8397(4) 0.9501(4) -0.0715(3) 0.0238(15) Uani 1 1 d . . . H15 H 0.8533 0.8887 -0.0597 0.029 Uiso 1 1 calc R . . C16 C 0.8037(5) 0.9846(5) -0.1207(2) 0.0272(16) Uani 1 1 d . . . H16 H 0.7933 0.9460 -0.1424 0.033 Uiso 1 1 calc R . . C17 C 0.7819(4) 1.0750(5) -0.1396(2) 0.0245(15) Uani 1 1 d . . . C18 C 0.8009(4) 1.1304(4) -0.1072(2) 0.0211(15) Uani 1 1 d . . . H18 H 0.7898 1.1908 -0.1197 0.025 Uiso 1 1 calc R . . C19 C 0.8357(4) 1.0963(4) -0.0576(2) 0.0187(14) Uani 1 1 d . . . H19 H 0.8457 1.1350 -0.0358 0.022 Uiso 1 1 calc R . . C20 C 0.8962(4) 0.9754(4) 0.4850(2) 0.0195(14) Uani 1 1 d . . . C21 C 0.8604(4) 1.0030(4) 0.5357(2) 0.0195(14) Uani 1 1 d . . . C22 C 0.8442(4) 1.0897(4) 0.5509(2) 0.0204(14) Uani 1 1 d . . . H22 H 0.8533 1.1322 0.5270 0.025 Uiso 1 1 calc R . . C23 C 0.8153(4) 1.1136(4) 0.5998(2) 0.0212(15) Uani 1 1 d . . . H23 H 0.8044 1.1725 0.6088 0.025 Uiso 1 1 calc R . . C24 C 0.8018(4) 1.0521(5) 0.6368(2) 0.0247(15) Uani 1 1 d . . . C25 C 0.8180(4) 0.9649(4) 0.6215(3) 0.0236(15) Uani 1 1 d . . . H25 H 0.8099 0.9217 0.6454 0.028 Uiso 1 1 calc R . . C26 C 0.8454(4) 0.9427(4) 0.5723(2) 0.0201(14) Uani 1 1 d . . . H26 H 0.8544 0.8847 0.5627 0.024 Uiso 1 1 calc R . . C27 C 0.9572(4) 0.8794(4) 0.4811(2) 0.0220(15) Uani 1 1 d . . . C28 C 1.0188(4) 0.8229(4) 0.5221(2) 0.0220(15) Uani 1 1 d . . . H28 H 1.0189 0.8485 0.5534 0.026 Uiso 1 1 calc R . . C29 C 1.0778(4) 0.7329(4) 0.5182(2) 0.0209(15) Uani 1 1 d . . . H29 H 1.1180 0.6979 0.5467 0.025 Uiso 1 1 calc R . . C30 C 1.0802(4) 0.6905(5) 0.4725(3) 0.0260(16) Uani 1 1 d . . . C31 C 1.0198(4) 0.7462(5) 0.4306(3) 0.0269(16) Uani 1 1 d . . . H31 H 1.0203 0.7206 0.3993 0.032 Uiso 1 1 calc R . . C32 C 0.9616(4) 0.8357(5) 0.4349(2) 0.0250(15) Uani 1 1 d . . . H32 H 0.9221 0.8709 0.4063 0.030 Uiso 1 1 calc R . . C33 C 0.8726(4) 1.0428(4) 0.4411(2) 0.0203(14) Uani 1 1 d . . . C34 C 0.9338(4) 1.0299(4) 0.3990(2) 0.0181(14) Uani 1 1 d . . . H34 H 0.9901 0.9752 0.4000 0.022 Uiso 1 1 calc R . . C35 C 0.9143(5) 1.0927(4) 0.3577(2) 0.0250(15) Uani 1 1 d . . . H35 H 0.9574 1.0816 0.3309 0.030 Uiso 1 1 calc R . . C36 C 0.8294(4) 1.1756(4) 0.3541(2) 0.0221(15) Uani 1 1 d . . . C37 C 0.7691(5) 1.1884(4) 0.3957(2) 0.0255(16) Uani 1 1 d . . . H37 H 0.7126 1.2430 0.3948 0.031 Uiso 1 1 calc R . . C38 C 0.7896(4) 1.1246(4) 0.4371(2) 0.0181(14) Uani 1 1 d . . . H38 H 0.7466 1.1358 0.4640 0.022 Uiso 1 1 calc R . . C39 C 0.3660(4) 0.0405(4) 0.4883(2) 0.0209(14) Uani 1 1 d . . . C40 C 0.3591(4) 0.0016(4) 0.5402(2) 0.0210(15) Uani 1 1 d . . . C41 C 0.2916(4) 0.0562(5) 0.5738(2) 0.0242(15) Uani 1 1 d . . . H41 H 0.2510 0.1180 0.5626 0.029 Uiso 1 1 calc R . . C42 C 0.2842(5) 0.0204(4) 0.6229(2) 0.0231(15) Uani 1 1 d . . . H42 H 0.2378 0.0579 0.6445 0.028 Uiso 1 1 calc R . . C43 C 0.3443(5) -0.0711(5) 0.6414(2) 0.0251(16) Uani 1 1 d . . . C44 C 0.4133(5) -0.1244(4) 0.6085(2) 0.0247(15) Uani 1 1 d . . . H44 H 0.4567 -0.1849 0.6204 0.030 Uiso 1 1 calc R . . C45 C 0.4183(4) -0.0897(4) 0.5594(2) 0.0207(14) Uani 1 1 d . . . H45 H 0.4632 -0.1283 0.5375 0.025 Uiso 1 1 calc R . . C46 C 0.3963(4) -0.0174(4) 0.4466(2) 0.0189(14) Uani 1 1 d . . . C47 C 0.3863(4) -0.0997(4) 0.4466(2) 0.0214(15) Uani 1 1 d . . . H47 H 0.3579 -0.1166 0.4750 0.026 Uiso 1 1 calc R . . C48 C 0.4153(4) -0.1552(4) 0.4078(2) 0.0227(15) Uani 1 1 d . . . H48 H 0.4074 -0.2097 0.4099 0.027 Uiso 1 1 calc R . . C49 C 0.4573(4) -0.1329(5) 0.3643(2) 0.0247(15) Uani 1 1 d . . . C50 C 0.4694(4) -0.0515(5) 0.3631(3) 0.0259(16) Uani 1 1 d . . . H50 H 0.4989 -0.0356 0.3348 0.031 Uiso 1 1 calc R . . C51 C 0.4389(4) 0.0044(5) 0.4026(2) 0.0233(15) Uani 1 1 d . . . H51 H 0.4464 0.0591 0.4005 0.028 Uiso 1 1 calc R . . C52 C 0.3444(4) 0.1361(4) 0.4808(2) 0.0207(14) Uani 1 1 d . . . C53 C 0.3057(4) 0.1903(4) 0.4332(2) 0.0247(15) Uani 1 1 d . . . H53 H 0.2887 0.1640 0.4065 0.030 Uiso 1 1 calc R . . C54 C 0.2925(5) 0.2792(4) 0.4251(2) 0.0268(16) Uani 1 1 d . . . H54 H 0.2653 0.3136 0.3934 0.032 Uiso 1 1 calc R . . C55 C 0.3188(4) 0.3209(4) 0.4634(2) 0.0224(15) Uani 1 1 d . . . C56 C 0.3557(4) 0.2690(4) 0.5114(2) 0.0233(15) Uani 1 1 d . . . H56 H 0.3725 0.2952 0.5382 0.028 Uiso 1 1 calc R . . C57 C 0.3671(4) 0.1793(4) 0.5185(2) 0.0210(14) Uani 1 1 d . . . H57 H 0.3916 0.1455 0.5508 0.025 Uiso 1 1 calc R . . C58 C 0.3786(4) 0.0180(4) 0.0196(2) 0.0219(15) Uani 1 1 d . . . C59 C 0.4183(4) -0.0510(4) 0.0621(2) 0.0180(14) Uani 1 1 d . . . C60 C 0.4752(4) -0.0424(4) 0.1011(2) 0.0241(15) Uani 1 1 d . . . H60 H 0.4841 0.0115 0.0991 0.029 Uiso 1 1 calc R . . C61 C 0.5168(5) -0.1069(4) 0.1405(2) 0.0235(15) Uani 1 1 d . . . H61 H 0.5538 -0.0976 0.1654 0.028 Uiso 1 1 calc R . . C62 C 0.5054(4) -0.1901(4) 0.1451(2) 0.0213(15) Uani 1 1 d . . . C63 C 0.4484(5) -0.1992(5) 0.1070(2) 0.0262(16) Uani 1 1 d . . . H63 H 0.4379 -0.2523 0.1093 0.031 Uiso 1 1 calc R . . C64 C 0.4080(4) -0.1327(4) 0.0669(2) 0.0218(15) Uiso 1 1 d . . . H64 H 0.3719 -0.1421 0.0414 0.026 Uiso 1 1 calc R . . C65 C 0.3632(4) -0.0043(4) -0.0307(2) 0.0217(15) Uani 1 1 d . . . C66 C 0.4221(4) -0.0918(4) -0.0483(2) 0.0220(15) Uani 1 1 d . . . H66 H 0.4677 -0.1370 -0.0250 0.026 Uiso 1 1 calc R . . C67 C 0.4150(4) -0.1126(4) -0.0971(2) 0.0229(15) Uani 1 1 d . . . H67 H 0.4563 -0.1710 -0.1071 0.027 Uiso 1 1 calc R . . C68 C 0.3470(4) -0.0484(4) -0.1331(2) 0.0201(14) Uani 1 1 d . . . C69 C 0.2874(4) 0.0389(4) -0.1160(2) 0.0227(15) Uani 1 1 d . . . H69 H 0.2407 0.0837 -0.1389 0.027 Uiso 1 1 calc R . . C70 C 0.2967(5) 0.0584(4) -0.0673(2) 0.0232(15) Uani 1 1 d . . . H70 H 0.2563 0.1173 -0.0575 0.028 Uiso 1 1 calc R . . C71 C 0.3538(4) 0.1138(4) 0.0270(2) 0.0223(15) Uani 1 1 d . . . C72 C 0.3589(4) 0.1752(4) -0.0120(2) 0.0232(15) Uani 1 1 d . . . H72 H 0.3728 0.1562 -0.0457 0.028 Uiso 1 1 calc R . . C73 C 0.3446(5) 0.2635(4) -0.0037(3) 0.0261(16) Uani 1 1 d . . . H73 H 0.3491 0.3032 -0.0313 0.031 Uiso 1 1 calc R . . C74 C 0.3231(5) 0.2937(5) 0.0465(3) 0.0292(16) Uani 1 1 d . . . C75 C 0.3137(5) 0.2332(5) 0.0859(2) 0.0263(16) Uani 1 1 d . . . H75 H 0.2967 0.2532 0.1192 0.032 Uiso 1 1 calc R . . C76 C 0.3287(5) 0.1461(4) 0.0769(3) 0.0245(15) Uani 1 1 d . . . H76 H 0.3224 0.1067 0.1041 0.029 Uiso 1 1 calc R . . C77 C 0.3328(5) 0.6440(5) 0.4775(3) 0.0384(19) Uiso 1 1 d . . . H77A H 0.3316 0.6131 0.4472 0.058 Uiso 1 1 calc R . . H77B H 0.2950 0.7101 0.4702 0.058 Uiso 1 1 calc R . . H77C H 0.3076 0.6212 0.5068 0.058 Uiso 1 1 calc R . . C78 C 0.4470(6) 0.6496(6) 0.5399(3) 0.047(2) Uiso 1 1 d . . . H78A H 0.5142 0.6231 0.5463 0.071 Uiso 1 1 calc R . . H78B H 0.4192 0.6253 0.5671 0.071 Uiso 1 1 calc R . . H78C H 0.4203 0.7163 0.5396 0.071 Uiso 1 1 calc R . . C79 C 0.4981(5) 0.5843(5) 0.4584(3) 0.0268(16) Uiso 1 1 d . . . H79 H 0.4831 0.5677 0.4270 0.032 Uiso 1 1 calc R . . C80 C -0.0565(8) 0.3148(8) 0.1635(5) 0.092(4) Uiso 1 1 d . . . H80A H -0.0474 0.3640 0.1437 0.139 Uiso 1 1 calc R . . H80B H -0.1033 0.3408 0.1893 0.139 Uiso 1 1 calc R . . H80C H -0.0775 0.2834 0.1401 0.139 Uiso 1 1 calc R . . C81 C 0.1164(7) 0.2557(8) 0.1722(4) 0.084(3) Uiso 1 1 d . . . H81A H 0.1194 0.2557 0.1347 0.125 Uiso 1 1 calc R . . H81B H 0.1710 0.2031 0.1883 0.125 Uiso 1 1 calc R . . H81C H 0.1154 0.3124 0.1823 0.125 Uiso 1 1 calc R . . C82 C 0.0355(6) 0.1852(6) 0.2260(3) 0.047(2) Uiso 1 1 d . . . H82 H 0.0946 0.1453 0.2413 0.056 Uiso 1 1 calc R . . C83 C -0.0542(5) 0.1657(6) 0.7910(3) 0.044(2) Uiso 1 1 d . . . H83A H -0.0279 0.1640 0.8250 0.066 Uiso 1 1 calc R . . H83B H -0.0938 0.1339 0.7940 0.066 Uiso 1 1 calc R . . H83C H -0.0913 0.2294 0.7773 0.066 Uiso 1 1 calc R . . C84 C -0.0077(6) 0.1228(6) 0.7030(3) 0.051(2) Uiso 1 1 d . . . H84A H 0.0475 0.0960 0.6823 0.077 Uiso 1 1 calc R . . H84B H -0.0462 0.1863 0.6893 0.077 Uiso 1 1 calc R . . H84C H -0.0436 0.0875 0.7015 0.077 Uiso 1 1 calc R . . C85 C 0.1065(5) 0.0814(6) 0.7720(3) 0.045(2) Uiso 1 1 d . . . H85 H 0.1178 0.0831 0.8075 0.054 Uiso 1 1 calc R . . C86 C 0.3842(7) 0.6131(7) 1.0504(4) 0.075(3) Uiso 1 1 d . . . H86A H 0.3388 0.6756 1.0555 0.112 Uiso 1 1 calc R . . H86B H 0.4414 0.5977 1.0703 0.112 Uiso 1 1 calc R . . H86C H 0.3586 0.5703 1.0619 0.112 Uiso 1 1 calc R . . C87 C 0.4497(6) 0.6542(6) 0.9723(3) 0.052(2) Uiso 1 1 d . . . H87A H 0.4460 0.6510 0.9351 0.077 Uiso 1 1 calc R . . H87B H 0.5149 0.6262 0.9841 0.077 Uiso 1 1 calc R . . H87C H 0.4199 0.7184 0.9798 0.077 Uiso 1 1 calc R . . C88 C 0.3633(6) 0.5641(6) 0.9704(4) 0.057(2) Uiso 1 1 d . . . H88 H 0.3729 0.5632 0.9344 0.068 Uiso 1 1 calc R . . C89 C 0.5427(9) 0.8820(10) 0.7688(5) 0.118(5) Uiso 1 1 d . . . H89A H 0.5574 0.8258 0.7913 0.176 Uiso 1 1 calc R . . H89B H 0.5048 0.8839 0.7391 0.176 Uiso 1 1 calc R . . H89C H 0.5082 0.9353 0.7879 0.176 Uiso 1 1 calc R . . C90 C 0.6906(9) 0.8088(10) 0.7248(6) 0.124(5) Uiso 1 1 d . . . H90A H 0.7303 0.8284 0.7036 0.186 Uiso 1 1 calc R . . H90B H 0.6554 0.7886 0.7028 0.186 Uiso 1 1 calc R . . H90C H 0.7291 0.7580 0.7499 0.186 Uiso 1 1 calc R . . C91 C 0.6495(7) 0.9504(7) 0.7639(4) 0.068(3) Uiso 1 1 d . . . H91 H 0.6027 0.9983 0.7806 0.081 Uiso 1 1 calc R . . C92 C 0.2695(9) 0.3165(9) 0.6685(5) 0.117(5) Uiso 1 1 d . . . H92A H 0.2195 0.3785 0.6696 0.175 Uiso 1 1 calc R . . H92B H 0.2838 0.3042 0.6325 0.175 Uiso 1 1 calc R . . H92C H 0.3250 0.3113 0.6867 0.175 Uiso 1 1 calc R . . C93 C 0.1466(6) 0.2612(6) 0.6777(4) 0.059(3) Uiso 1 1 d . . . H93A H 0.1383 0.2076 0.6916 0.089 Uiso 1 1 calc R . . H93B H 0.1407 0.2672 0.6400 0.089 Uiso 1 1 calc R . . H93C H 0.0991 0.3163 0.6910 0.089 Uiso 1 1 calc R . . C94 C 0.2944(6) 0.1851(6) 0.7281(3) 0.047(2) Uiso 1 1 d . . . H94 H 0.2710 0.1450 0.7436 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0430(4) 0.0215(3) 0.0220(3) -0.0071(3) 0.0096(3) -0.0106(3) Mo2 0.0447(4) 0.0172(3) 0.0184(3) -0.0095(3) 0.0083(3) -0.0110(3) Mo3 0.0309(3) 0.0176(3) 0.0198(3) -0.0074(2) 0.0021(3) -0.0075(3) Mo4 0.0403(4) 0.0148(3) 0.0148(3) -0.0028(2) 0.0000(3) -0.0094(3) Mo5 0.0428(4) 0.0294(4) 0.0178(3) -0.0104(3) 0.0012(3) -0.0162(3) Mo6 0.0356(4) 0.0133(3) 0.0134(3) -0.0044(2) 0.0039(2) -0.0079(3) Mo7 0.0299(3) 0.0157(3) 0.0194(3) -0.0091(2) -0.0005(2) -0.0072(3) Mo8 0.0343(4) 0.0218(3) 0.0190(3) -0.0079(3) 0.0027(3) -0.0116(3) O1 0.062(4) 0.043(3) 0.035(3) -0.012(3) 0.022(3) -0.024(3) O2 0.046(3) 0.034(3) 0.036(3) -0.015(3) 0.014(2) -0.007(3) O3 0.034(3) 0.021(3) 0.030(3) -0.009(2) 0.008(2) -0.009(2) O4 0.051(3) 0.026(3) 0.019(2) 0.000(2) 0.003(2) -0.019(2) O5 0.057(3) 0.019(3) 0.023(3) -0.012(2) 0.012(2) -0.016(2) O6 0.062(4) 0.027(3) 0.024(3) -0.016(2) 0.010(2) -0.018(3) O7 0.051(3) 0.023(3) 0.029(3) -0.008(2) 0.014(2) -0.013(2) O8 0.034(3) 0.015(2) 0.021(2) -0.0048(19) 0.002(2) -0.009(2) O9 0.033(3) 0.021(3) 0.032(3) -0.008(2) 0.006(2) -0.005(2) O10 0.033(3) 0.029(3) 0.030(3) -0.016(2) 0.002(2) -0.015(2) O11 0.040(3) 0.012(2) 0.020(2) -0.0077(19) 0.005(2) -0.008(2) O12 0.050(3) 0.024(3) 0.026(3) -0.002(2) -0.003(2) -0.014(2) O13 0.044(3) 0.025(3) 0.017(2) -0.010(2) 0.002(2) -0.016(2) O14 0.068(4) 0.053(4) 0.030(3) -0.028(3) 0.011(3) -0.037(3) O15 0.045(3) 0.015(2) 0.024(3) -0.008(2) 0.007(2) -0.013(2) O16 0.038(3) 0.018(2) 0.028(3) -0.003(2) 0.004(2) -0.005(2) O17 0.031(3) 0.016(2) 0.025(2) -0.008(2) 0.007(2) -0.010(2) O18 0.036(3) 0.018(2) 0.026(3) -0.015(2) -0.003(2) -0.005(2) O19 0.034(3) 0.019(2) 0.033(3) -0.008(2) -0.002(2) -0.008(2) O20 0.037(3) 0.016(2) 0.014(2) -0.0085(19) 0.0002(19) -0.009(2) O21 0.050(3) 0.032(3) 0.031(3) -0.002(2) -0.004(2) -0.015(3) O22 0.045(3) 0.022(3) 0.021(2) -0.011(2) 0.001(2) -0.016(2) O23 0.044(3) 0.021(3) 0.015(2) -0.004(2) 0.005(2) -0.011(2) O24 0.031(3) 0.024(3) 0.019(2) -0.013(2) 0.004(2) -0.010(2) O25 0.036(3) 0.032(3) 0.037(3) -0.010(2) -0.003(2) -0.014(2) O26 0.042(3) 0.034(3) 0.024(3) -0.013(2) 0.010(2) -0.018(2) O32 0.051(4) 0.067(4) 0.027(3) -0.008(3) 0.002(3) -0.027(3) N1 0.048(4) 0.041(4) 0.052(4) -0.033(4) 0.004(3) -0.010(3) N3 0.059(4) 0.022(3) 0.020(3) -0.002(3) -0.003(3) -0.019(3) N4 0.049(4) 0.023(3) 0.017(3) -0.007(3) 0.010(3) -0.016(3) N5 0.042(4) 0.016(3) 0.030(3) -0.006(3) 0.000(3) -0.004(3) N6 0.040(4) 0.023(3) 0.023(3) -0.001(3) 0.013(3) 0.000(3) N7 0.053(4) 0.016(3) 0.022(3) -0.006(3) 0.004(3) -0.015(3) N8 0.052(4) 0.032(4) 0.030(3) -0.016(3) 0.014(3) -0.018(3) N9 0.042(4) 0.016(3) 0.022(3) -0.004(2) -0.006(3) -0.011(3) N10 0.056(4) 0.020(3) 0.034(4) 0.006(3) -0.013(3) -0.020(3) N11 0.036(3) 0.024(3) 0.024(3) -0.010(3) 0.002(3) -0.009(3) N12 0.066(4) 0.016(3) 0.023(3) -0.013(3) 0.007(3) -0.014(3) C1 0.028(4) 0.017(3) 0.018(3) -0.001(3) 0.001(3) -0.010(3) C2 0.024(4) 0.021(4) 0.014(3) -0.002(3) 0.001(3) -0.005(3) C3 0.027(4) 0.019(4) 0.027(4) -0.002(3) 0.000(3) -0.010(3) C4 0.023(4) 0.024(4) 0.030(4) -0.006(3) 0.000(3) -0.007(3) C5 0.042(5) 0.031(4) 0.035(4) -0.022(4) 0.014(4) -0.017(4) C6 0.039(4) 0.039(5) 0.018(4) 0.000(3) 0.000(3) -0.017(4) C7 0.034(4) 0.027(4) 0.010(3) -0.008(3) 0.005(3) -0.011(3) C8 0.024(4) 0.022(4) 0.021(3) -0.004(3) 0.001(3) -0.007(3) C9 0.040(4) 0.021(4) 0.023(4) -0.005(3) 0.009(3) -0.001(3) C10 0.060(5) 0.030(4) 0.015(4) 0.005(3) 0.006(4) 0.002(4) C11 0.059(6) 0.018(4) 0.044(5) 0.007(4) 0.006(4) 0.012(4) C12 0.060(5) 0.024(4) 0.019(4) -0.003(3) 0.010(4) -0.004(4) C13 0.034(4) 0.025(4) 0.014(3) -0.010(3) 0.009(3) -0.011(3) C14 0.015(3) 0.024(4) 0.013(3) -0.008(3) 0.000(3) 0.000(3) C15 0.025(4) 0.013(3) 0.030(4) -0.008(3) 0.002(3) -0.004(3) C16 0.035(4) 0.028(4) 0.017(3) -0.003(3) 0.000(3) -0.012(3) C17 0.026(4) 0.026(4) 0.020(3) -0.008(3) 0.006(3) -0.008(3) C18 0.019(3) 0.017(3) 0.020(3) 0.001(3) 0.004(3) -0.003(3) C19 0.020(3) 0.010(3) 0.022(3) -0.009(3) 0.005(3) -0.002(3) C20 0.017(3) 0.021(4) 0.019(3) -0.007(3) -0.003(3) -0.006(3) C21 0.021(3) 0.017(3) 0.019(3) -0.008(3) 0.000(3) -0.006(3) C22 0.023(4) 0.019(3) 0.018(3) -0.001(3) 0.001(3) -0.010(3) C23 0.027(4) 0.016(3) 0.017(3) -0.008(3) -0.001(3) -0.005(3) C24 0.020(4) 0.031(4) 0.023(4) -0.011(3) 0.002(3) -0.010(3) C25 0.027(4) 0.016(3) 0.027(4) -0.006(3) 0.001(3) -0.007(3) C26 0.020(3) 0.014(3) 0.024(4) -0.010(3) 0.002(3) -0.005(3) C27 0.031(4) 0.021(4) 0.020(3) -0.014(3) 0.008(3) -0.014(3) C28 0.034(4) 0.023(4) 0.013(3) -0.009(3) 0.000(3) -0.015(3) C29 0.026(4) 0.021(4) 0.012(3) -0.006(3) 0.002(3) -0.006(3) C30 0.024(4) 0.023(4) 0.031(4) -0.010(3) 0.006(3) -0.010(3) C31 0.031(4) 0.031(4) 0.021(4) -0.013(3) 0.003(3) -0.013(3) C32 0.027(4) 0.028(4) 0.021(3) -0.007(3) -0.004(3) -0.011(3) C33 0.021(3) 0.024(4) 0.021(3) -0.012(3) 0.001(3) -0.012(3) C34 0.020(3) 0.018(3) 0.015(3) -0.007(3) -0.006(3) -0.005(3) C35 0.033(4) 0.027(4) 0.013(3) -0.012(3) 0.002(3) -0.011(3) C36 0.029(4) 0.018(3) 0.016(3) -0.004(3) -0.003(3) -0.007(3) C37 0.033(4) 0.016(3) 0.025(4) -0.008(3) 0.004(3) -0.007(3) C38 0.021(3) 0.021(3) 0.012(3) -0.009(3) 0.001(3) -0.008(3) C39 0.025(4) 0.019(3) 0.019(3) -0.006(3) 0.000(3) -0.009(3) C40 0.027(4) 0.021(4) 0.018(3) -0.007(3) -0.005(3) -0.012(3) C41 0.027(4) 0.026(4) 0.025(4) -0.008(3) -0.001(3) -0.016(3) C42 0.031(4) 0.022(4) 0.022(4) -0.008(3) 0.007(3) -0.015(3) C43 0.031(4) 0.031(4) 0.020(4) -0.008(3) -0.002(3) -0.019(3) C44 0.034(4) 0.015(3) 0.027(4) -0.001(3) -0.006(3) -0.012(3) C45 0.030(4) 0.024(4) 0.013(3) -0.004(3) -0.004(3) -0.015(3) C46 0.020(3) 0.020(3) 0.017(3) -0.004(3) -0.004(3) -0.009(3) C47 0.028(4) 0.028(4) 0.014(3) -0.004(3) 0.002(3) -0.017(3) C48 0.030(4) 0.023(4) 0.022(4) -0.001(3) -0.009(3) -0.018(3) C49 0.025(4) 0.023(4) 0.025(4) -0.014(3) -0.002(3) -0.007(3) C50 0.028(4) 0.029(4) 0.022(4) -0.008(3) -0.001(3) -0.012(3) C51 0.031(4) 0.022(4) 0.017(3) -0.001(3) -0.005(3) -0.011(3) C52 0.028(4) 0.020(4) 0.020(3) -0.001(3) -0.004(3) -0.016(3) C53 0.035(4) 0.025(4) 0.016(3) -0.009(3) 0.003(3) -0.013(3) C54 0.041(4) 0.019(4) 0.018(3) -0.003(3) -0.004(3) -0.010(3) C55 0.031(4) 0.015(3) 0.020(3) -0.005(3) 0.002(3) -0.009(3) C56 0.034(4) 0.021(4) 0.019(3) -0.010(3) 0.003(3) -0.014(3) C57 0.028(4) 0.019(3) 0.014(3) -0.003(3) -0.003(3) -0.009(3) C58 0.026(4) 0.020(4) 0.025(4) -0.013(3) 0.008(3) -0.013(3) C59 0.029(4) 0.009(3) 0.016(3) -0.005(3) 0.004(3) -0.009(3) C60 0.031(4) 0.022(4) 0.024(4) -0.012(3) 0.009(3) -0.014(3) C61 0.040(4) 0.026(4) 0.012(3) -0.006(3) -0.003(3) -0.020(3) C62 0.022(3) 0.023(4) 0.018(3) -0.012(3) 0.006(3) -0.006(3) C63 0.036(4) 0.021(4) 0.028(4) -0.007(3) 0.002(3) -0.017(3) C65 0.027(4) 0.015(3) 0.024(4) -0.005(3) 0.002(3) -0.009(3) C66 0.026(4) 0.019(4) 0.021(3) -0.005(3) -0.002(3) -0.010(3) C67 0.029(4) 0.015(3) 0.024(4) -0.015(3) 0.009(3) -0.006(3) C68 0.027(4) 0.024(4) 0.018(3) -0.007(3) 0.003(3) -0.018(3) C69 0.025(4) 0.019(4) 0.022(4) -0.005(3) 0.002(3) -0.008(3) C70 0.036(4) 0.014(3) 0.021(3) -0.011(3) 0.006(3) -0.010(3) C71 0.027(4) 0.018(3) 0.024(4) -0.017(3) 0.006(3) -0.010(3) C72 0.035(4) 0.015(3) 0.017(3) -0.011(3) 0.005(3) -0.007(3) C73 0.039(4) 0.020(4) 0.020(3) -0.007(3) 0.002(3) -0.013(3) C74 0.041(4) 0.028(4) 0.022(4) -0.014(3) 0.005(3) -0.016(3) C75 0.039(4) 0.029(4) 0.015(3) -0.008(3) 0.003(3) -0.017(3) C76 0.037(4) 0.019(4) 0.022(4) -0.008(3) 0.003(3) -0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.692(5) . ? Mo1 O2 1.710(5) . ? Mo1 O3 1.920(5) . ? Mo1 O5 1.941(5) . ? Mo1 O4 2.273(5) . ? Mo1 O8 2.488(4) . ? Mo2 O7 1.710(5) . ? Mo2 O6 1.718(5) . ? Mo2 O5 1.904(5) . ? Mo2 O15 2.005(4) . ? Mo2 O8 2.306(4) . ? Mo2 O13 2.343(5) . ? Mo3 O9 1.712(4) . ? Mo3 O10 1.715(4) . ? Mo3 O3 1.912(4) . ? Mo3 O17 2.009(4) . ? Mo3 O11 2.334(4) . ? Mo3 O8 2.348(4) . ? Mo4 O12 1.701(5) . ? Mo4 O4 1.768(5) . ? Mo4 O11 1.942(4) . ? Mo4 O13 1.946(4) . ? Mo4 O20 2.155(4) . ? Mo4 O8 2.346(4) . ? Mo5 O21 1.708(5) . ? Mo5 O14 1.710(5) . ? Mo5 O22 1.889(4) . ? Mo5 O13 2.012(4) . ? Mo5 O20 2.323(4) . ? Mo5 O15 2.333(5) . ? Mo6 O16 1.701(4) . ? Mo6 O23 1.761(4) . ? Mo6 O17 1.951(4) . ? Mo6 O15 1.955(5) . ? Mo6 O8 2.164(4) . ? Mo6 O20 2.375(4) . ? Mo7 O18 1.696(4) . ? Mo7 O19 1.715(4) . ? Mo7 O24 1.895(4) . ? Mo7 O11 2.011(4) . ? Mo7 O20 2.309(4) . ? Mo7 O17 2.351(4) . ? Mo8 O25 1.701(5) . ? Mo8 O26 1.717(4) . ? Mo8 O22 1.930(4) . ? Mo8 O24 1.942(4) . ? Mo8 O23 2.318(5) . ? Mo8 O20 2.490(4) . ? O27 C79 1.218(7) . ? O28 C82 1.221(8) . ? O29 C85 1.274(9) . ? O30 C88 1.247(9) . ? O31 C91 1.193(10) . ? O32 C94 1.225(9) . ? N1 C5 1.338(9) . ? N1 H1A 0.8800 . ? N1 H1B 0.8800 . ? N2 C11 1.371(10) . ? N2 H2A 0.8800 . ? N2 H2B 0.8800 . ? N3 C17 1.358(8) . ? N3 H3A 0.8800 . ? N3 H3B 0.8800 . ? N4 C24 1.349(8) . ? N4 H4A 0.8800 . ? N4 H4B 0.8800 . ? N5 C30 1.349(8) . ? N5 H5A 0.8800 . ? N5 H5B 0.8800 . ? N6 C36 1.327(8) . ? N6 H6A 0.8800 . ? N6 H6B 0.8800 . ? N7 C43 1.336(8) . ? N7 H7A 0.8800 . ? N7 H7B 0.8800 . ? N8 C49 1.339(8) . ? N8 H8A 0.8800 . ? N8 H8B 0.8800 . ? N9 C55 1.340(8) . ? N9 H9A 0.8800 . ? N9 H9B 0.8800 . ? N10 C62 1.347(8) . ? N10 H10A 0.8800 . ? N10 H10B 0.8800 . ? N11 C68 1.343(8) . ? N11 H11A 0.8800 . ? N11 H11B 0.8800 . ? N12 C74 1.343(8) . ? N12 H12A 0.8800 . ? N12 H12B 0.8800 . ? N13 C79 1.349(8) . ? N13 C77 1.452(8) . ? N13 C78 1.467(10) . ? N14 C82 1.337(10) . ? N14 C80 1.467(12) . ? N14 C81 1.472(11) . ? N15 C85 1.291(9) . ? N15 C83 1.456(9) . ? N15 C84 1.461(10) . ? N16 C88 1.385(11) . ? N16 C86 1.399(11) . ? N16 C87 1.417(10) . ? N17 C91 1.356(12) . ? N17 C90 1.425(14) . ? N17 C89 1.444(13) . ? N18 C94 1.318(10) . ? N18 C92 1.476(13) . ? N18 C93 1.477(10) . ? C1 C2 1.433(9) . ? C1 C14 1.459(8) . ? C1 C8 1.468(9) . ? C2 C7 1.427(9) . ? C2 C3 1.444(9) . ? C3 C4 1.365(9) . ? C3 H3 0.9500 . ? C4 C5 1.412(10) . ? C4 H4 0.9500 . ? C5 C6 1.411(10) . ? C6 C7 1.369(9) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.413(9) . ? C8 C13 1.421(8) . ? C9 C10 1.389(9) . ? C9 H9 0.9500 . ? C10 C11 1.407(10) . ? C10 H10 0.9500 . ? C11 C12 1.415(10) . ? C12 C13 1.340(9) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.410(9) . ? C14 C15 1.419(9) . ? C15 C16 1.378(9) . ? C15 H15 0.9500 . ? C16 C17 1.403(9) . ? C16 H16 0.9500 . ? C17 C18 1.416(9) . ? C18 C19 1.384(8) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C33 1.445(9) . ? C20 C27 1.450(9) . ? C20 C21 1.467(8) . ? C21 C26 1.405(8) . ? C21 C22 1.416(9) . ? C22 C23 1.384(8) . ? C22 H22 0.9500 . ? C23 C24 1.416(9) . ? C23 H23 0.9500 . ? C24 C25 1.425(9) . ? C25 C26 1.382(9) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C28 1.420(9) . ? C27 C32 1.439(9) . ? C28 C29 1.367(9) . ? C28 H28 0.9500 . ? C29 C30 1.423(9) . ? C29 H29 0.9500 . ? C30 C31 1.426(9) . ? C31 C32 1.360(9) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.409(8) . ? C33 C34 1.433(8) . ? C34 C35 1.356(8) . ? C34 H34 0.9500 . ? C35 C36 1.434(9) . ? C35 H35 0.9500 . ? C36 C37 1.414(9) . ? C37 C38 1.368(8) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C52 1.438(9) . ? C39 C46 1.442(9) . ? C39 C40 1.470(8) . ? C40 C41 1.417(9) . ? C40 C45 1.417(9) . ? C41 C42 1.386(9) . ? C41 H41 0.9500 . ? C42 C43 1.418(9) . ? C42 H42 0.9500 . ? C43 C44 1.409(9) . ? C44 C45 1.369(8) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.423(9) . ? C46 C51 1.428(8) . ? C47 C48 1.359(9) . ? C47 H47 0.9500 . ? C48 C49 1.415(9) . ? C48 H48 0.9500 . ? C49 C50 1.424(9) . ? C50 C51 1.378(9) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? C52 C57 1.399(9) . ? C52 C53 1.432(8) . ? C53 C54 1.369(9) . ? C53 H53 0.9500 . ? C54 C55 1.422(9) . ? C54 H54 0.9500 . ? C55 C56 1.421(9) . ? C56 C57 1.391(9) . ? C56 H56 0.9500 . ? C57 H57 0.9500 . ? C58 C59 1.439(8) . ? C58 C65 1.443(9) . ? C58 C71 1.467(8) . ? C59 C64 1.411(8) . ? C59 C60 1.428(9) . ? C60 C61 1.349(9) . ? C60 H60 0.9500 . ? C61 C62 1.444(9) . ? C61 H61 0.9500 . ? C62 C63 1.418(9) . ? C63 C64 1.374(9) . ? C63 H63 0.9500 . ? C64 H64 0.9500 . ? C65 C70 1.409(9) . ? C65 C66 1.437(9) . ? C66 C67 1.365(9) . ? C66 H66 0.9500 . ? C67 C68 1.419(9) . ? C67 H67 0.9500 . ? C68 C69 1.433(9) . ? C69 C70 1.363(9) . ? C69 H69 0.9500 . ? C70 H70 0.9500 . ? C71 C72 1.394(9) . ? C71 C76 1.434(9) . ? C72 C73 1.393(9) . ? C72 H72 0.9500 . ? C73 C74 1.426(9) . ? C73 H73 0.9500 . ? C74 C75 1.416(9) . ? C75 C76 1.378(9) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79 0.9500 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82 0.9500 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 H85 0.9500 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88 0.9500 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C91 H91 0.9500 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 H94 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Mo1 O2 104.5(2) . . ? O1 Mo1 O3 103.5(2) . . ? O2 Mo1 O3 98.4(2) . . ? O1 Mo1 O5 102.8(2) . . ? O2 Mo1 O5 98.4(2) . . ? O3 Mo1 O5 143.90(19) . . ? O1 Mo1 O4 91.8(2) . . ? O2 Mo1 O4 163.64(19) . . ? O3 Mo1 O4 76.98(18) . . ? O5 Mo1 O4 77.94(19) . . ? O1 Mo1 O8 160.9(2) . . ? O2 Mo1 O8 94.58(19) . . ? O3 Mo1 O8 74.14(17) . . ? O5 Mo1 O8 72.85(16) . . ? O4 Mo1 O8 69.08(14) . . ? O7 Mo2 O6 103.9(2) . . ? O7 Mo2 O5 101.5(2) . . ? O6 Mo2 O5 100.7(2) . . ? O7 Mo2 O15 97.2(2) . . ? O6 Mo2 O15 100.3(2) . . ? O5 Mo2 O15 147.50(18) . . ? O7 Mo2 O8 97.3(2) . . ? O6 Mo2 O8 158.6(2) . . ? O5 Mo2 O8 77.95(17) . . ? O15 Mo2 O8 73.48(17) . . ? O7 Mo2 O13 165.65(19) . . ? O6 Mo2 O13 86.8(2) . . ? O5 Mo2 O13 85.61(18) . . ? O15 Mo2 O13 71.09(16) . . ? O8 Mo2 O13 71.80(15) . . ? O9 Mo3 O10 105.4(2) . . ? O9 Mo3 O3 101.9(2) . . ? O10 Mo3 O3 101.4(2) . . ? O9 Mo3 O17 97.7(2) . . ? O10 Mo3 O17 99.92(19) . . ? O3 Mo3 O17 145.9(2) . . ? O9 Mo3 O11 162.7(2) . . ? O10 Mo3 O11 90.21(19) . . ? O3 Mo3 O11 81.93(17) . . ? O17 Mo3 O11 71.61(16) . . ? O9 Mo3 O8 93.8(2) . . ? O10 Mo3 O8 160.45(19) . . ? O3 Mo3 O8 77.77(18) . . ? O17 Mo3 O8 73.29(16) . . ? O11 Mo3 O8 70.28(15) . . ? O12 Mo4 O4 105.4(2) . . ? O12 Mo4 O11 100.7(2) . . ? O4 Mo4 O11 95.5(2) . . ? O12 Mo4 O13 101.7(2) . . ? O4 Mo4 O13 98.1(2) . . ? O11 Mo4 O13 149.62(18) . . ? O12 Mo4 O20 97.7(2) . . ? O4 Mo4 O20 156.82(19) . . ? O11 Mo4 O20 78.46(17) . . ? O13 Mo4 O20 78.37(17) . . ? O12 Mo4 O8 173.57(19) . . ? O4 Mo4 O8 80.92(18) . . ? O11 Mo4 O8 77.24(16) . . ? O13 Mo4 O8 78.27(17) . . ? O20 Mo4 O8 75.93(15) . . ? O21 Mo5 O14 105.0(3) . . ? O21 Mo5 O22 101.4(2) . . ? O14 Mo5 O22 101.6(2) . . ? O21 Mo5 O13 96.5(2) . . ? O14 Mo5 O13 100.2(2) . . ? O22 Mo5 O13 146.97(19) . . ? O21 Mo5 O20 94.1(2) . . ? O14 Mo5 O20 160.5(2) . . ? O22 Mo5 O20 78.08(17) . . ? O13 Mo5 O20 73.17(16) . . ? O21 Mo5 O15 163.1(2) . . ? O14 Mo5 O15 88.9(2) . . ? O22 Mo5 O15 84.65(18) . . ? O13 Mo5 O15 71.20(17) . . ? O20 Mo5 O15 71.61(15) . . ? O16 Mo6 O23 106.0(2) . . ? O16 Mo6 O17 100.9(2) . . ? O23 Mo6 O17 95.96(19) . . ? O16 Mo6 O15 101.5(2) . . ? O23 Mo6 O15 97.6(2) . . ? O17 Mo6 O15 149.31(18) . . ? O16 Mo6 O8 97.73(19) . . ? O23 Mo6 O8 156.26(18) . . ? O17 Mo6 O8 78.73(17) . . ? O15 Mo6 O8 77.76(17) . . ? O16 Mo6 O20 172.88(18) . . ? O23 Mo6 O20 81.11(17) . . ? O17 Mo6 O20 77.81(16) . . ? O15 Mo6 O20 77.30(16) . . ? O8 Mo6 O20 75.15(15) . . ? O18 Mo7 O19 104.0(2) . . ? O18 Mo7 O24 100.4(2) . . ? O19 Mo7 O24 102.7(2) . . ? O18 Mo7 O11 99.7(2) . . ? O19 Mo7 O11 97.2(2) . . ? O24 Mo7 O11 147.17(18) . . ? O18 Mo7 O20 159.59(18) . . ? O19 Mo7 O20 95.97(19) . . ? O24 Mo7 O20 78.63(17) . . ? O11 Mo7 O20 73.53(17) . . ? O18 Mo7 O17 87.68(18) . . ? O19 Mo7 O17 164.97(19) . . ? O24 Mo7 O17 83.95(17) . . ? O11 Mo7 O17 71.22(16) . . ? O20 Mo7 O17 71.92(15) . . ? O25 Mo8 O26 104.8(2) . . ? O25 Mo8 O22 99.3(2) . . ? O26 Mo8 O22 104.2(2) . . ? O25 Mo8 O24 99.1(2) . . ? O26 Mo8 O24 101.4(2) . . ? O22 Mo8 O24 143.28(19) . . ? O25 Mo8 O23 165.63(19) . . ? O26 Mo8 O23 89.59(19) . . ? O22 Mo8 O23 77.21(18) . . ? O24 Mo8 O23 77.09(17) . . ? O25 Mo8 O20 96.57(19) . . ? O26 Mo8 O20 158.60(19) . . ? O22 Mo8 O20 73.24(17) . . ? O24 Mo8 O20 73.31(16) . . ? O23 Mo8 O20 69.06(14) . . ? Mo3 O3 Mo1 116.7(2) . . ? Mo4 O4 Mo1 118.1(2) . . ? Mo2 O5 Mo1 117.8(2) . . ? Mo6 O8 Mo2 92.36(16) . . ? Mo6 O8 Mo4 104.80(17) . . ? Mo2 O8 Mo4 97.65(16) . . ? Mo6 O8 Mo3 91.39(15) . . ? Mo2 O8 Mo3 162.3(2) . . ? Mo4 O8 Mo3 98.11(16) . . ? Mo6 O8 Mo1 163.2(2) . . ? Mo2 O8 Mo1 86.66(14) . . ? Mo4 O8 Mo1 91.90(14) . . ? Mo3 O8 Mo1 84.78(14) . . ? Mo4 O11 Mo7 108.6(2) . . ? Mo4 O11 Mo3 111.68(19) . . ? Mo7 O11 Mo3 104.33(18) . . ? Mo4 O13 Mo5 109.6(2) . . ? Mo4 O13 Mo2 109.1(2) . . ? Mo5 O13 Mo2 104.32(18) . . ? Mo6 O15 Mo2 109.2(2) . . ? Mo6 O15 Mo5 110.45(19) . . ? Mo2 O15 Mo5 104.92(18) . . ? Mo6 O17 Mo3 109.3(2) . . ? Mo6 O17 Mo7 109.9(2) . . ? Mo3 O17 Mo7 103.77(17) . . ? Mo4 O20 Mo7 91.96(16) . . ? Mo4 O20 Mo5 92.43(15) . . ? Mo7 O20 Mo5 162.8(2) . . ? Mo4 O20 Mo6 104.11(17) . . ? Mo7 O20 Mo6 97.74(15) . . ? Mo5 O20 Mo6 97.34(15) . . ? Mo4 O20 Mo8 163.8(2) . . ? Mo7 O20 Mo8 85.77(13) . . ? Mo5 O20 Mo8 85.37(14) . . ? Mo6 O20 Mo8 92.10(14) . . ? Mo5 O22 Mo8 117.6(2) . . ? Mo6 O23 Mo8 117.7(2) . . ? Mo7 O24 Mo8 116.8(2) . . ? C5 N1 H1A 120.0 . . ? C5 N1 H1B 120.0 . . ? H1A N1 H1B 120.0 . . ? C11 N2 H2A 120.0 . . ? C11 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C17 N3 H3A 120.0 . . ? C17 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? C24 N4 H4A 120.0 . . ? C24 N4 H4B 120.0 . . ? H4A N4 H4B 120.0 . . ? C30 N5 H5A 120.0 . . ? C30 N5 H5B 120.0 . . ? H5A N5 H5B 120.0 . . ? C36 N6 H6A 120.0 . . ? C36 N6 H6B 120.0 . . ? H6A N6 H6B 120.0 . . ? C43 N7 H7A 120.0 . . ? C43 N7 H7B 120.0 . . ? H7A N7 H7B 120.0 . . ? C49 N8 H8A 120.0 . . ? C49 N8 H8B 120.0 . . ? H8A N8 H8B 120.0 . . ? C55 N9 H9A 120.0 . . ? C55 N9 H9B 120.0 . . ? H9A N9 H9B 120.0 . . ? C62 N10 H10A 120.0 . . ? C62 N10 H10B 120.0 . . ? H10A N10 H10B 120.0 . . ? C68 N11 H11A 120.0 . . ? C68 N11 H11B 120.0 . . ? H11A N11 H11B 120.0 . . ? C74 N12 H12A 120.0 . . ? C74 N12 H12B 120.0 . . ? H12A N12 H12B 120.0 . . ? C79 N13 C77 122.4(6) . . ? C79 N13 C78 119.8(6) . . ? C77 N13 C78 117.7(6) . . ? C82 N14 C80 121.8(8) . . ? C82 N14 C81 121.0(8) . . ? C80 N14 C81 117.3(8) . . ? C85 N15 C83 121.7(7) . . ? C85 N15 C84 122.4(7) . . ? C83 N15 C84 115.9(6) . . ? C88 N16 C86 117.3(8) . . ? C88 N16 C87 120.2(8) . . ? C86 N16 C87 121.7(8) . . ? C91 N17 C90 121.6(9) . . ? C91 N17 C89 119.7(9) . . ? C90 N17 C89 118.4(10) . . ? C94 N18 C92 120.0(8) . . ? C94 N18 C93 123.7(7) . . ? C92 N18 C93 116.3(8) . . ? C2 C1 C14 121.4(6) . . ? C2 C1 C8 119.9(6) . . ? C14 C1 C8 118.7(6) . . ? C7 C2 C1 122.1(6) . . ? C7 C2 C3 116.1(6) . . ? C1 C2 C3 121.8(6) . . ? C4 C3 C2 120.9(6) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 121.7(6) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? N1 C5 C6 120.8(7) . . ? N1 C5 C4 120.9(7) . . ? C6 C5 C4 118.3(6) . . ? C7 C6 C5 120.4(7) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C2 122.4(6) . . ? C6 C7 H7 118.8 . . ? C2 C7 H7 118.8 . . ? C9 C8 C13 117.8(6) . . ? C9 C8 C1 120.0(6) . . ? C13 C8 C1 122.0(6) . . ? C10 C9 C8 120.6(6) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 119.8(6) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? N2 C11 C10 119.0(7) . . ? N2 C11 C12 121.6(8) . . ? C10 C11 C12 119.4(6) . . ? C13 C12 C11 120.3(7) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C8 122.0(6) . . ? C12 C13 H13 119.0 . . ? C8 C13 H13 119.0 . . ? C19 C14 C15 117.7(6) . . ? C19 C14 C1 120.7(6) . . ? C15 C14 C1 121.6(6) . . ? C16 C15 C14 120.4(6) . . ? C16 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? C15 C16 C17 121.8(7) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 119.1 . . ? N3 C17 C16 120.5(6) . . ? N3 C17 C18 121.3(6) . . ? C16 C17 C18 118.2(6) . . ? C19 C18 C17 119.9(6) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C14 121.9(6) . . ? C18 C19 H19 119.0 . . ? C14 C19 H19 119.0 . . ? C33 C20 C27 121.9(6) . . ? C33 C20 C21 120.4(5) . . ? C27 C20 C21 117.7(5) . . ? C26 C21 C22 117.3(5) . . ? C26 C21 C20 121.4(6) . . ? C22 C21 C20 121.2(6) . . ? C23 C22 C21 121.1(6) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C24 121.4(6) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? N4 C24 C23 122.1(6) . . ? N4 C24 C25 120.5(6) . . ? C23 C24 C25 117.4(6) . . ? C26 C25 C24 120.4(6) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C21 122.3(6) . . ? C25 C26 H26 118.8 . . ? C21 C26 H26 118.8 . . ? C28 C27 C32 115.5(6) . . ? C28 C27 C20 122.1(6) . . ? C32 C27 C20 122.3(6) . . ? C29 C28 C27 122.3(6) . . ? C29 C28 H28 118.8 . . ? C27 C28 H28 118.8 . . ? C28 C29 C30 121.4(6) . . ? C28 C29 H29 119.3 . . ? C30 C29 H29 119.3 . . ? N5 C30 C29 120.9(6) . . ? N5 C30 C31 121.8(6) . . ? C29 C30 C31 117.2(6) . . ? C32 C31 C30 120.8(6) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C31 C32 C27 122.8(6) . . ? C31 C32 H32 118.6 . . ? C27 C32 H32 118.6 . . ? C38 C33 C34 116.2(6) . . ? C38 C33 C20 122.6(5) . . ? C34 C33 C20 121.2(6) . . ? C35 C34 C33 122.6(6) . . ? C35 C34 H34 118.7 . . ? C33 C34 H34 118.7 . . ? C34 C35 C36 120.6(6) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? N6 C36 C37 122.0(6) . . ? N6 C36 C35 121.2(6) . . ? C37 C36 C35 116.8(6) . . ? C38 C37 C36 122.0(6) . . ? C38 C37 H37 119.0 . . ? C36 C37 H37 119.0 . . ? C37 C38 C33 121.8(6) . . ? C37 C38 H38 119.1 . . ? C33 C38 H38 119.1 . . ? C52 C39 C46 121.5(6) . . ? C52 C39 C40 118.4(6) . . ? C46 C39 C40 120.1(6) . . ? C41 C40 C45 117.0(6) . . ? C41 C40 C39 120.0(6) . . ? C45 C40 C39 123.0(6) . . ? C42 C41 C40 120.6(6) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C41 C42 C43 121.4(6) . . ? C41 C42 H42 119.3 . . ? C43 C42 H42 119.3 . . ? N7 C43 C44 122.3(6) . . ? N7 C43 C42 119.9(6) . . ? C44 C43 C42 117.8(6) . . ? C45 C44 C43 120.5(6) . . ? C45 C44 H44 119.7 . . ? C43 C44 H44 119.7 . . ? C44 C45 C40 122.5(6) . . ? C44 C45 H45 118.7 . . ? C40 C45 H45 118.7 . . ? C47 C46 C51 115.6(6) . . ? C47 C46 C39 122.5(6) . . ? C51 C46 C39 121.8(6) . . ? C48 C47 C46 123.1(6) . . ? C48 C47 H47 118.5 . . ? C46 C47 H47 118.5 . . ? C47 C48 C49 120.8(6) . . ? C47 C48 H48 119.6 . . ? C49 C48 H48 119.6 . . ? N8 C49 C48 121.6(6) . . ? N8 C49 C50 120.5(6) . . ? C48 C49 C50 117.8(6) . . ? C51 C50 C49 120.6(6) . . ? C51 C50 H50 119.7 . . ? C49 C50 H50 119.7 . . ? C50 C51 C46 122.0(6) . . ? C50 C51 H51 119.0 . . ? C46 C51 H51 119.0 . . ? C57 C52 C53 116.2(6) . . ? C57 C52 C39 121.3(6) . . ? C53 C52 C39 122.3(6) . . ? C54 C53 C52 121.6(6) . . ? C54 C53 H53 119.2 . . ? C52 C53 H53 119.2 . . ? C53 C54 C55 121.3(6) . . ? C53 C54 H54 119.4 . . ? C55 C54 H54 119.4 . . ? N9 C55 C56 119.7(6) . . ? N9 C55 C54 122.2(6) . . ? C56 C55 C54 118.1(6) . . ? C57 C56 C55 119.1(6) . . ? C57 C56 H56 120.4 . . ? C55 C56 H56 120.4 . . ? C56 C57 C52 123.6(6) . . ? C56 C57 H57 118.2 . . ? C52 C57 H57 118.2 . . ? C59 C58 C65 121.9(6) . . ? C59 C58 C71 119.3(6) . . ? C65 C58 C71 118.7(6) . . ? C64 C59 C60 115.9(6) . . ? C64 C59 C58 122.8(6) . . ? C60 C59 C58 121.3(6) . . ? C61 C60 C59 123.3(6) . . ? C61 C60 H60 118.3 . . ? C59 C60 H60 118.3 . . ? C60 C61 C62 120.4(6) . . ? C60 C61 H61 119.8 . . ? C62 C61 H61 119.8 . . ? N10 C62 C63 122.7(6) . . ? N10 C62 C61 120.4(6) . . ? C63 C62 C61 116.9(6) . . ? C64 C63 C62 121.3(6) . . ? C64 C63 H63 119.3 . . ? C62 C63 H63 119.3 . . ? C63 C64 C59 122.2(6) . . ? C63 C64 H64 118.9 . . ? C59 C64 H64 118.9 . . ? C70 C65 C66 115.2(6) . . ? C70 C65 C58 123.8(6) . . ? C66 C65 C58 120.8(6) . . ? C67 C66 C65 122.6(6) . . ? C67 C66 H66 118.7 . . ? C65 C66 H66 118.7 . . ? C66 C67 C68 121.1(6) . . ? C66 C67 H67 119.4 . . ? C68 C67 H67 119.4 . . ? N11 C68 C67 121.5(6) . . ? N11 C68 C69 121.5(6) . . ? C67 C68 C69 116.9(6) . . ? C70 C69 C68 120.8(6) . . ? C70 C69 H69 119.6 . . ? C68 C69 H69 119.6 . . ? C69 C70 C65 123.4(6) . . ? C69 C70 H70 118.3 . . ? C65 C70 H70 118.3 . . ? C72 C71 C76 117.2(6) . . ? C72 C71 C58 122.6(5) . . ? C76 C71 C58 120.0(6) . . ? C73 C72 C71 122.7(6) . . ? C73 C72 H72 118.6 . . ? C71 C72 H72 118.6 . . ? C72 C73 C74 119.6(6) . . ? C72 C73 H73 120.2 . . ? C74 C73 H73 120.2 . . ? N12 C74 C75 121.3(6) . . ? N12 C74 C73 120.6(6) . . ? C75 C74 C73 118.1(6) . . ? C76 C75 C74 121.3(6) . . ? C76 C75 H75 119.3 . . ? C74 C75 H75 119.3 . . ? C75 C76 C71 120.9(6) . . ? C75 C76 H76 119.5 . . ? C71 C76 H76 119.5 . . ? N13 C77 H77A 109.5 . . ? N13 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? N13 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? N13 C78 H78A 109.5 . . ? N13 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? N13 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? O27 C79 N13 125.8(7) . . ? O27 C79 H79 117.1 . . ? N13 C79 H79 117.1 . . ? N14 C80 H80A 109.5 . . ? N14 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? N14 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? N14 C81 H81A 109.5 . . ? N14 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? N14 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? O28 C82 N14 124.9(8) . . ? O28 C82 H82 117.5 . . ? N14 C82 H82 117.5 . . ? N15 C83 H83A 109.5 . . ? N15 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? N15 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? N15 C84 H84A 109.5 . . ? N15 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? N15 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? O29 C85 N15 128.0(8) . . ? O29 C85 H85 116.0 . . ? N15 C85 H85 116.0 . . ? N16 C86 H86A 109.5 . . ? N16 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? N16 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? N16 C87 H87A 109.5 . . ? N16 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? N16 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? O30 C88 N16 124.7(9) . . ? O30 C88 H88 117.6 . . ? N16 C88 H88 117.6 . . ? N17 C89 H89A 109.5 . . ? N17 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? N17 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? N17 C90 H90A 109.5 . . ? N17 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? N17 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? O31 C91 N17 128.5(10) . . ? O31 C91 H91 115.7 . . ? N17 C91 H91 115.7 . . ? N18 C92 H92A 109.5 . . ? N18 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? N18 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? N18 C93 H93A 109.5 . . ? N18 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? N18 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? O32 C94 N18 127.2(8) . . ? O32 C94 H94 116.4 . . ? N18 C94 H94 116.4 . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 2.492 _refine_diff_density_min -1.326 _refine_diff_density_rms 0.162 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 648023' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C114 H110 Co N18 O41 W12' _chemical_formula_weight 4653.33 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' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 29.4200(8) _cell_length_b 29.4200(8) _cell_length_c 12.6652(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 9493.5(6) _cell_formula_units_Z 3 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 6 _cell_measurement_theta_max 12 _exptl_crystal_description polyhedron _exptl_crystal_colour black _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6489 _exptl_absorpt_coefficient_mu 11.069 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.139 _exptl_absorpt_correction_T_max 0.193 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16784 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 24.99 _reflns_number_total 3712 _reflns_number_gt 3616 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SMART (Siemens, 1996)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990) ; _refine_special_details ; The anion is disordered around a site of -3 symmetry, which coincides with the position of the Co centre. This disorder results in site occupancies of 0.5 being assigned to most of the oxygen centres of the anion. The metal centres and some oxygen centres were found to be common to both superimposed orientations of the anion and were refined with full site occupancies. 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^)+(0.0000P)^2^+468.6000P] 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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3712 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0486 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1048 _refine_ls_wR_factor_gt 0.1044 _refine_ls_goodness_of_fit_ref 1.515 _refine_ls_restrained_S_all 1.515 _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 W1 W 0.38203(2) 0.802955(18) 0.16793(4) 0.03270(15) Uani 1 1 d . . . W2 W 0.31888(2) 0.72699(2) 0.38958(4) 0.03417(16) Uani 1 1 d . . . Co1 Co 0.3333 0.6667 0.1667 0.0190(7) Uani 1 6 d S . . O1 O 0.4041(4) 0.8678(3) 0.1657(8) 0.048(2) Uani 1 1 d . A . O2 O 0.3121(4) 0.7559(4) 0.4993(7) 0.047(2) Uani 1 1 d . A . O3A O 0.4578(6) 0.8185(6) 0.1848(11) 0.023(2) Uiso 0.50 1 d P A 1 O4A O 0.3981(5) 0.8079(6) 0.0083(11) 0.020(2) Uiso 0.50 1 d P A 1 O5A O 0.3642(6) 0.8000(6) 0.3244(11) 0.023(2) Uiso 0.50 1 d P A 1 O6A O 0.3804(6) 0.7248(6) 0.4661(12) 0.024(2) Uiso 0.50 1 d P . 1 O3B O 0.4328(6) 0.7881(6) 0.1977(11) 0.023(2) Uiso 0.50 1 d P A 2 O4B O 0.3755(5) 0.7767(6) 0.0324(11) 0.020(2) Uiso 0.50 1 d P A 2 O5B O 0.3666(6) 0.7758(6) 0.3008(11) 0.023(2) Uiso 0.50 1 d P A 2 O6B O 0.3788(6) 0.7226(6) 0.3974(12) 0.024(2) Uiso 0.50 1 d P . 2 O7 O 0.3333 0.6667 0.3157(17) 0.015(5) Uani 0.50 3 d SP . . O8 O 0.3869(5) 0.7329(5) 0.1197(11) 0.017(3) Uani 0.50 1 d P A . N1 N 0.4336(5) 0.7916(4) 0.6094(8) 0.047(3) Uani 1 1 d . . . H1A H 0.4298 0.7882 0.6768 0.056 Uiso 1 1 calc R . . H1B H 0.4177 0.7646 0.5692 0.056 Uiso 1 1 calc R . . N2 N 0.5412(6) 1.0678(7) 0.0517(12) 0.085(5) Uani 1 1 d . . . H2A H 0.5113 1.0544 0.0203 0.102 Uiso 1 1 calc R . . H2B H 0.5682 1.0943 0.0244 0.102 Uiso 1 1 calc R . . N3 N 0.7119(5) 1.1269(5) 0.7404(11) 0.064(4) Uani 1 1 d . . . H3A H 0.7302 1.1168 0.7760 0.077 Uiso 1 1 calc R . . H3B H 0.7155 1.1573 0.7516 0.077 Uiso 1 1 calc R . . C1 C 0.4633(5) 0.8378(5) 0.5684(9) 0.034(3) Uani 1 1 d . . . C2 C 0.4696(4) 0.8454(4) 0.4576(8) 0.027(2) Uani 1 1 d . . . H2 H 0.4524 0.8168 0.4123 0.033 Uiso 1 1 calc R . . C3 C 0.5012(4) 0.8947(4) 0.4172(8) 0.026(2) Uani 1 1 d . . . H3 H 0.5042 0.8988 0.3442 0.031 Uiso 1 1 calc R . . C4 C 0.5294(5) 0.9394(5) 0.4814(9) 0.031(3) Uani 1 1 d . . . C5 C 0.5212(5) 0.9301(5) 0.5930(9) 0.035(3) Uani 1 1 d . . . H5 H 0.5385 0.9584 0.6388 0.042 Uiso 1 1 calc R . . C6 C 0.4892(5) 0.8820(5) 0.6346(9) 0.034(3) Uani 1 1 d . . . H6 H 0.4844 0.8781 0.7073 0.041 Uiso 1 1 calc R . . C7 C 0.5625(4) 0.9910(4) 0.4430(10) 0.032(3) Uani 1 1 d . . . C8 C 0.5555(4) 1.0075(4) 0.3403(10) 0.033(3) Uani 1 1 d . . . C9 C 0.5073(5) 0.9850(4) 0.2849(10) 0.031(3) Uani 1 1 d . . . H9 H 0.4782 0.9561 0.3139 0.037 Uiso 1 1 calc R . . C10 C 0.5023(5) 1.0042(5) 0.1909(11) 0.040(3) Uani 1 1 d . . . H10 H 0.4699 0.9886 0.1572 0.049 Uiso 1 1 calc R . . C11 C 0.5457(6) 1.0474(6) 0.1443(12) 0.050(4) Uani 1 1 d . . . C12 C 0.5940(5) 1.0706(6) 0.1981(12) 0.053(4) Uani 1 1 d . . . H12 H 0.6232 1.0994 0.1690 0.063 Uiso 1 1 calc R . . C13 C 0.5982(5) 1.0510(5) 0.2922(12) 0.045(3) Uani 1 1 d . . . H13 H 0.6306 1.0669 0.3262 0.054 Uiso 1 1 calc R . . C14 C 0.6036(5) 1.0273(5) 0.5135(11) 0.042(3) Uani 1 1 d . . . C15 C 0.6132(5) 1.0790(5) 0.5294(10) 0.036(3) Uani 1 1 d . . . H15 H 0.5954 1.0912 0.4880 0.043 Uiso 1 1 calc R . . C16 C 0.6479(5) 1.1115(5) 0.6043(10) 0.043(3) Uani 1 1 d . . . H16 H 0.6527 1.1449 0.6153 0.051 Uiso 1 1 calc R . . C17 C 0.6764(5) 1.0937(6) 0.6646(12) 0.053(4) Uani 1 1 d . . . C18 C 0.6698(6) 1.0448(7) 0.6450(15) 0.068(5) Uani 1 1 d . . . H18 H 0.6899 1.0337 0.6815 0.082 Uiso 1 1 calc R . . C19 C 0.6339(6) 1.0126(6) 0.5721(13) 0.056(4) Uani 1 1 d . . . H19 H 0.6297 0.9795 0.5613 0.068 Uiso 1 1 calc R . . O9 O 0.3333 0.6667 0.6667 0.074(8) Uiso 1 6 d S . . 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 W1 0.0453(3) 0.0169(2) 0.0353(3) -0.00242(19) -0.0085(2) 0.0151(2) W2 0.0367(3) 0.0372(3) 0.0259(3) -0.0138(2) 0.0051(2) 0.0165(2) Co1 0.0199(10) 0.0199(10) 0.0172(16) 0.000 0.000 0.0099(5) O1 0.065(6) 0.024(4) 0.052(6) -0.003(4) -0.026(5) 0.019(4) O2 0.048(5) 0.050(6) 0.036(5) -0.021(4) 0.010(4) 0.018(5) O7 0.015(7) 0.015(7) 0.016(11) 0.000 0.000 0.007(3) O8 0.015(7) 0.010(6) 0.022(7) 0.003(5) 0.007(5) 0.003(5) N1 0.058(7) 0.040(6) 0.026(6) 0.011(5) 0.001(5) 0.012(6) N2 0.056(9) 0.114(13) 0.073(10) 0.057(10) 0.013(8) 0.034(9) N3 0.046(7) 0.066(9) 0.069(9) -0.030(7) -0.024(7) 0.020(7) C1 0.042(7) 0.040(7) 0.031(6) 0.003(5) 0.005(5) 0.029(6) C2 0.028(6) 0.028(6) 0.021(6) -0.004(5) -0.003(5) 0.010(5) C3 0.029(6) 0.030(6) 0.021(5) 0.008(4) 0.002(4) 0.017(5) C4 0.036(7) 0.032(6) 0.028(6) 0.003(5) -0.004(5) 0.020(5) C5 0.046(7) 0.038(7) 0.031(6) -0.007(5) -0.006(6) 0.028(6) C6 0.052(8) 0.047(7) 0.015(5) -0.004(5) -0.003(5) 0.033(7) C7 0.021(6) 0.026(6) 0.050(8) 0.004(5) -0.001(5) 0.011(5) C8 0.023(6) 0.026(6) 0.052(8) 0.004(5) 0.008(5) 0.013(5) C9 0.029(6) 0.023(6) 0.041(7) 0.004(5) 0.008(5) 0.013(5) C10 0.033(7) 0.043(8) 0.049(8) 0.009(6) 0.006(6) 0.022(6) C11 0.048(8) 0.053(9) 0.047(8) 0.019(7) 0.009(7) 0.025(7) C12 0.034(7) 0.049(9) 0.064(10) 0.025(7) 0.013(7) 0.013(7) C13 0.029(7) 0.034(7) 0.066(10) 0.007(7) 0.010(6) 0.012(6) C14 0.038(7) 0.033(7) 0.056(9) -0.005(6) -0.011(6) 0.018(6) C15 0.029(6) 0.030(6) 0.042(7) -0.001(5) -0.005(5) 0.009(5) C16 0.029(7) 0.041(8) 0.044(8) -0.006(6) 0.007(6) 0.007(6) C17 0.028(7) 0.054(9) 0.057(9) -0.010(7) 0.000(6) 0.006(7) C18 0.044(9) 0.056(10) 0.103(14) -0.006(9) -0.033(9) 0.024(8) C19 0.052(9) 0.033(7) 0.087(12) -0.008(7) -0.029(8) 0.024(7) _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 W1 O1 1.680(8) . ? W1 O3B 1.794(14) . ? W1 O5B 1.820(14) . ? W1 O3B 1.847(14) 15 ? W1 O4B 1.852(14) . ? W1 O5A 2.040(14) . ? W1 O3A 2.051(14) . ? W1 O4A 2.065(14) . ? W1 O3A 2.100(14) 15 ? W1 O8 2.222(13) . ? W1 O8 2.263(13) 15 ? W2 O2 1.693(8) . ? W2 O4B 1.782(14) 15 ? W2 O5B 1.812(14) . ? W2 O6B 1.815(14) 2_665 ? W2 O6B 1.833(14) . ? W2 O5A 2.052(14) . ? W2 O4A 2.063(14) 15 ? W2 O6A 2.074(15) 2_665 ? W2 O6A 2.083(15) . ? W2 O7 2.227(9) . ? W2 O8 2.240(13) 15 ? Co1 O7 1.89(2) 13_565 ? Co1 O7 1.89(2) . ? Co1 O8 1.888(12) 14_455 ? Co1 O8 1.888(12) 2_665 ? Co1 O8 1.888(12) 13_565 ? Co1 O8 1.888(12) . ? Co1 O8 1.888(12) 3_565 ? Co1 O8 1.888(12) 15 ? O3A W1 2.100(14) 14_455 ? O4A W2 2.063(14) 14_455 ? O6A W2 2.074(15) 3_565 ? O3B O8 1.801(19) . ? O3B W1 1.846(14) 14_455 ? O4B W2 1.782(13) 14_455 ? O6B W2 1.815(14) 3_565 ? O7 W2 2.227(9) 2_665 ? O7 W2 2.227(9) 3_565 ? O8 W2 2.240(13) 14_455 ? O8 W1 2.263(13) 14_455 ? N1 C1 1.301(16) . ? N1 H1A 0.8600 . ? N1 H1B 0.8600 . ? N2 C11 1.354(18) . ? N2 H2A 0.8600 . ? N2 H2B 0.8600 . ? N3 C17 1.395(18) . ? N3 H3A 0.8600 . ? N3 H3B 0.8600 . ? C1 C6 1.408(17) . ? C1 C2 1.418(16) . ? C2 C3 1.372(15) . ? C2 H2 0.9300 . ? C3 C4 1.411(16) . ? C3 H3 0.9300 . ? C4 C7 1.417(16) . ? C4 C5 1.438(16) . ? C5 C6 1.354(18) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.438(17) . ? C7 C14 1.451(17) . ? C8 C13 1.408(17) . ? C8 C9 1.414(17) . ? C9 C10 1.358(17) . ? C9 H9 0.9300 . ? C10 C11 1.404(18) . ? C10 H10 0.9300 . ? C11 C12 1.41(2) . ? C12 C13 1.36(2) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C19 1.385(18) . ? C14 C15 1.416(17) . ? C15 C16 1.372(17) . ? C15 H15 0.9300 . ? C16 C17 1.41(2) . ? C16 H16 0.9300 . ? C17 C18 1.37(2) . ? C18 C19 1.37(2) . ? C18 H18 0.9300 . ? C19 H19 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 W1 O3B 112.5(6) . . ? O1 W1 O5B 112.6(6) . . ? O3B W1 O5B 75.8(7) . . ? O1 W1 O3B 110.2(6) . 15 ? O3B W1 O3B 137.3(9) . 15 ? O5B W1 O3B 89.3(6) . 15 ? O1 W1 O4B 111.0(5) . . ? O3B W1 O4B 91.0(6) . . ? O5B W1 O4B 136.3(7) . . ? O3B W1 O4B 72.5(6) 15 . ? O1 W1 O5A 90.6(5) . . ? O3B W1 O5A 90.7(6) . . ? O5B W1 O5A 23.2(5) . . ? O3B W1 O5A 90.0(6) 15 . ? O4B W1 O5A 155.7(6) . . ? O1 W1 O3A 89.3(5) . . ? O3B W1 O3A 24.1(5) . . ? O5B W1 O3A 90.4(6) . . ? O3B W1 O3A 159.0(7) 15 . ? O4B W1 O3A 93.6(6) . . ? O5A W1 O3A 97.8(6) . . ? O1 W1 O4A 87.6(5) . . ? O3B W1 O4A 92.0(6) . . ? O5B W1 O4A 159.1(6) . . ? O3B W1 O4A 88.6(6) 15 . ? O4B W1 O4A 25.1(5) . . ? O5A W1 O4A 177.2(6) . . ? O3A W1 O4A 84.3(5) . . ? O1 W1 O3A 87.8(5) . 15 ? O3B W1 O3A 158.9(7) . 15 ? O5B W1 O3A 91.4(6) . 15 ? O3B W1 O3A 23.5(5) 15 15 ? O4B W1 O3A 86.8(6) . 15 ? O5A W1 O3A 82.9(6) . 15 ? O3A W1 O3A 177.0(7) . 15 ? O4A W1 O3A 94.8(5) . 15 ? O1 W1 O8 151.7(5) . . ? O3B W1 O8 52.0(6) . . ? O5B W1 O8 88.0(6) . . ? O3B W1 O8 88.4(6) 15 . ? O4B W1 O8 53.1(5) . . ? O5A W1 O8 111.2(5) . . ? O3A W1 O8 70.6(5) . . ? O4A W1 O8 71.2(5) . . ? O3A W1 O8 111.9(5) 15 . ? O1 W1 O8 150.8(5) . 15 ? O3B W1 O8 89.9(6) . 15 ? O5B W1 O8 53.3(6) . 15 ? O3B W1 O8 50.8(5) 15 15 ? O4B W1 O8 85.9(6) . 15 ? O5A W1 O8 69.9(5) . 15 ? O3A W1 O8 114.0(5) . 15 ? O4A W1 O8 111.0(5) . 15 ? O3A W1 O8 69.0(5) 15 15 ? O8 W1 O8 57.3(6) . 15 ? O2 W2 O4B 111.1(6) . 15 ? O2 W2 O5B 110.5(6) . . ? O4B W2 O5B 93.7(6) 15 . ? O2 W2 O6B 110.6(6) . 2_665 ? O4B W2 O6B 72.8(6) 15 2_665 ? O5B W2 O6B 138.9(7) . 2_665 ? O2 W2 O6B 110.6(6) . . ? O4B W2 O6B 138.3(7) 15 . ? O5B W2 O6B 72.4(7) . . ? O6B W2 O6B 91.9(9) 2_665 . ? O2 W2 O5A 89.0(5) . . ? O4B W2 O5A 94.3(6) 15 . ? O5B W2 O5A 23.0(5) . . ? O6B W2 O5A 159.3(6) 2_665 . ? O6B W2 O5A 87.2(6) . . ? O2 W2 O4A 87.9(5) . 15 ? O4B W2 O4A 25.0(5) 15 15 ? O5B W2 O4A 93.7(6) . 15 ? O6B W2 O4A 89.2(6) 2_665 15 ? O6B W2 O4A 159.7(6) . 15 ? O5A W2 O4A 84.7(5) . 15 ? O2 W2 O6A 87.5(5) . 2_665 ? O4B W2 O6A 89.1(6) 15 2_665 ? O5B W2 O6A 159.2(6) . 2_665 ? O6B W2 O6A 24.8(5) 2_665 2_665 ? O6B W2 O6A 92.0(6) . 2_665 ? O5A W2 O6A 175.8(6) . 2_665 ? O4A W2 O6A 97.4(6) 15 2_665 ? O2 W2 O6A 87.5(5) . . ? O4B W2 O6A 159.0(6) 15 . ? O5B W2 O6A 88.4(6) . . ? O6B W2 O6A 92.0(6) 2_665 . ? O6B W2 O6A 24.7(5) . . ? O5A W2 O6A 95.7(6) . . ? O4A W2 O6A 175.3(6) 15 . ? O6A W2 O6A 82.0(8) 2_665 . ? O2 W2 O7 149.6(6) . . ? O4B W2 O7 89.3(6) 15 . ? O5B W2 O7 89.4(6) . . ? O6B W2 O7 52.8(5) 2_665 . ? O6B W2 O7 52.6(5) . . ? O5A W2 O7 112.4(6) . . ? O4A W2 O7 114.3(5) 15 . ? O6A W2 O7 70.0(5) 2_665 . ? O6A W2 O7 69.9(5) . . ? O2 W2 O8 151.1(5) . 15 ? O4B W2 O8 53.3(5) 15 15 ? O5B W2 O8 53.8(6) . 15 ? O6B W2 O8 89.1(6) 2_665 15 ? O6B W2 O8 88.9(6) . 15 ? O5A W2 O8 70.2(5) . 15 ? O4A W2 O8 70.9(5) 15 15 ? O6A W2 O8 113.9(5) 2_665 15 ? O6A W2 O8 113.6(5) . 15 ? O7 W2 O8 59.3(6) . 15 ? O7 Co1 O7 179.996(5) 13_565 . ? O7 Co1 O8 108.4(4) 13_565 14_455 ? O7 Co1 O8 71.6(4) . 14_455 ? O7 Co1 O8 71.6(4) 13_565 2_665 ? O7 Co1 O8 108.4(4) . 2_665 ? O8 Co1 O8 179.997(1) 14_455 2_665 ? O7 Co1 O8 108.4(4) 13_565 13_565 ? O7 Co1 O8 71.6(4) . 13_565 ? O8 Co1 O8 110.5(4) 14_455 13_565 ? O8 Co1 O8 69.5(4) 2_665 13_565 ? O7 Co1 O8 71.6(4) 13_565 . ? O7 Co1 O8 108.4(4) . . ? O8 Co1 O8 69.5(4) 14_455 . ? O8 Co1 O8 110.5(4) 2_665 . ? O8 Co1 O8 179.996(3) 13_565 . ? O7 Co1 O8 71.6(4) 13_565 3_565 ? O7 Co1 O8 108.4(4) . 3_565 ? O8 Co1 O8 69.5(4) 14_455 3_565 ? O8 Co1 O8 110.5(4) 2_665 3_565 ? O8 Co1 O8 69.5(4) 13_565 3_565 ? O8 Co1 O8 110.5(4) . 3_565 ? O7 Co1 O8 108.4(4) 13_565 15 ? O7 Co1 O8 71.6(4) . 15 ? O8 Co1 O8 110.5(4) 14_455 15 ? O8 Co1 O8 69.5(4) 2_665 15 ? O8 Co1 O8 110.5(4) 13_565 15 ? O8 Co1 O8 69.5(4) . 15 ? O8 Co1 O8 180.0(6) 3_565 15 ? W1 O3A W1 115.9(7) . 14_455 ? W2 O4A W1 114.6(7) 14_455 . ? W1 O5A W2 117.0(7) . . ? W2 O6A W2 114.7(7) 3_565 . ? W1 O3B O8 76.3(7) . . ? W1 O3B W1 150.4(9) . 14_455 ? O8 O3B W1 76.7(7) . 14_455 ? W2 O4B W1 145.9(8) 14_455 . ? W2 O5B W1 147.7(9) . . ? W2 O6B W2 147.3(9) 3_565 . ? Co1 O7 W2 114.8(5) . . ? Co1 O7 W2 114.8(5) . 2_665 ? W2 O7 W2 103.6(6) . 2_665 ? Co1 O7 W2 114.8(5) . 3_565 ? W2 O7 W2 103.6(6) . 3_565 ? W2 O7 W2 103.6(6) 2_665 3_565 ? O3B O8 Co1 128.3(9) . . ? O3B O8 W1 51.7(6) . . ? Co1 O8 W1 117.6(6) . . ? O3B O8 W2 117.4(8) . 14_455 ? Co1 O8 W2 114.3(6) . 14_455 ? W1 O8 W2 102.3(5) . 14_455 ? O3B O8 W1 52.6(6) . 14_455 ? Co1 O8 W1 115.6(6) . 14_455 ? W1 O8 W1 103.4(5) . 14_455 ? W2 O8 W1 101.6(5) 14_455 14_455 ? C1 N1 H1A 120.0 . . ? C1 N1 H1B 120.0 . . ? H1A N1 H1B 120.0 . . ? C11 N2 H2A 120.0 . . ? C11 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C17 N3 H3A 120.0 . . ? C17 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? N1 C1 C6 119.8(11) . . ? N1 C1 C2 121.7(12) . . ? C6 C1 C2 118.5(11) . . ? C3 C2 C1 120.1(11) . . ? C3 C2 H2 119.9 . . ? C1 C2 H2 119.9 . . ? C2 C3 C4 122.9(10) . . ? C2 C3 H3 118.6 . . ? C4 C3 H3 118.6 . . ? C3 C4 C7 124.7(11) . . ? C3 C4 C5 115.1(10) . . ? C7 C4 C5 120.1(11) . . ? C6 C5 C4 123.0(11) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C5 C6 C1 120.4(11) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C4 C7 C8 122.2(11) . . ? C4 C7 C14 116.8(11) . . ? C8 C7 C14 121.0(11) . . ? C13 C8 C9 116.2(12) . . ? C13 C8 C7 119.0(12) . . ? C9 C8 C7 124.8(10) . . ? C10 C9 C8 122.2(11) . . ? C10 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? C9 C10 C11 120.4(13) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? N2 C11 C10 121.3(14) . . ? N2 C11 C12 120.2(14) . . ? C10 C11 C12 118.4(13) . . ? C13 C12 C11 120.3(13) . . ? C13 C12 H12 119.9 . . ? C11 C12 H12 119.9 . . ? C12 C13 C8 122.5(13) . . ? C12 C13 H13 118.8 . . ? C8 C13 H13 118.8 . . ? C19 C14 C15 116.4(12) . . ? C19 C14 C7 122.0(12) . . ? C15 C14 C7 121.5(11) . . ? C16 C15 C14 121.8(13) . . ? C16 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? C15 C16 C17 119.2(13) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? C18 C17 N3 121.3(15) . . ? C18 C17 C16 119.4(14) . . ? N3 C17 C16 119.3(14) . . ? C19 C18 C17 120.2(14) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C14 122.8(14) . . ? C18 C19 H19 118.6 . . ? C14 C19 H19 118.6 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.257 _refine_diff_density_min -1.524 _refine_diff_density_rms 0.172 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 648024' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C114 H110 N18 O41 W12 Zn' _chemical_formula_weight 4659.77 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 29.4039(16) _cell_length_b 29.4039(16) _cell_length_c 12.6458(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 9468.6(12) _cell_formula_units_Z 3 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 6 _cell_measurement_theta_max 12 _exptl_crystal_description polyhedron _exptl_crystal_colour black-purple _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6498 _exptl_absorpt_coefficient_mu 11.157 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.106 _exptl_absorpt_correction_T_max 0.190 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(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 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16719 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3706 _reflns_number_gt 3682 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SMART (Siemens, 1996)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990) ; _refine_special_details ; The anion is disordered around a site of -3 symmetry, which coincides with the position of the Zn centre. This disorder results in site occupancies of 0.5 being assigned to most of the oxygen centres of the anion. The metal centres and some oxygen centres were found to be common to both superimposed orientations of the anion and were refined with full site occupancies. 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^)+(0.0000P)^2^+1609.1000P] 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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3706 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0797 _refine_ls_R_factor_gt 0.0794 _refine_ls_wR_factor_ref 0.1771 _refine_ls_wR_factor_gt 0.1770 _refine_ls_goodness_of_fit_ref 1.527 _refine_ls_restrained_S_all 1.527 _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 W1 W 0.38186(2) 0.80287(2) 0.16686(5) 0.03143(16) Uani 1 1 d . . . W2 W 0.31967(2) 0.72750(2) 0.38953(5) 0.03320(16) Uani 1 1 d . . . Zn1 Zn 0.3333 0.6667 0.1667 0.0227(8) Uani 1 6 d S . . O1 O 0.4044(4) 0.8681(4) 0.1652(10) 0.047(3) Uani 1 1 d . A . O2 O 0.3127(4) 0.7564(4) 0.5001(9) 0.045(3) Uani 1 1 d . A . O3A O 0.4586(6) 0.8192(6) 0.1834(14) 0.022(3) Uiso 0.50 1 d P A 1 O4A O 0.3988(6) 0.8081(6) 0.0064(13) 0.016(3) Uiso 0.50 1 d P A 1 O5A O 0.3645(6) 0.8001(6) 0.3246(14) 0.020(3) Uiso 0.50 1 d P A 1 O6A O 0.3808(7) 0.7249(7) 0.4667(15) 0.025(3) Uiso 0.50 1 d P . 1 O3B O 0.4337(6) 0.7892(7) 0.1968(14) 0.022(3) Uiso 0.50 1 d P A 2 O4B O 0.3763(6) 0.7770(6) 0.0333(13) 0.016(3) Uiso 0.50 1 d P A 2 O5B O 0.3670(6) 0.7761(7) 0.3005(14) 0.020(3) Uiso 0.50 1 d P A 2 O6B O 0.3786(7) 0.7225(7) 0.3975(15) 0.025(3) Uiso 0.50 1 d P . 2 O7 O 0.3333 0.6667 0.314(2) 0.013(6) Uani 0.50 3 d SP . . O8 O 0.3871(6) 0.7329(6) 0.1201(13) 0.018(4) Uani 0.50 1 d P A . N1 N 0.4345(6) 0.7920(5) 0.6099(11) 0.046(4) Uani 1 1 d . . . H1A H 0.4178 0.7642 0.5692 0.056 Uiso 1 1 calc R . . H1B H 0.4313 0.7887 0.6791 0.056 Uiso 1 1 calc R . . N2 N 0.5407(6) 1.0676(8) 0.0510(14) 0.087(6) Uani 1 1 d . . . H2A H 0.5680 1.0953 0.0235 0.104 Uiso 1 1 calc R . . H2B H 0.5102 1.0531 0.0181 0.104 Uiso 1 1 calc R . . N3 N 0.7117(6) 1.1267(7) 0.7412(15) 0.068(5) Uani 1 1 d . . . H3A H 0.7302 1.1163 0.7783 0.082 Uiso 1 1 calc R . . H3B H 0.7157 1.1581 0.7520 0.082 Uiso 1 1 calc R . . C1 C 0.4634(6) 0.8372(5) 0.5687(12) 0.034(4) Uani 1 1 d . . . C2 C 0.4700(5) 0.8449(5) 0.4580(11) 0.025(3) Uani 1 1 d . . . H2 H 0.4523 0.8159 0.4113 0.031 Uiso 1 1 calc R . . C3 C 0.5020(5) 0.8945(5) 0.4178(11) 0.022(3) Uani 1 1 d . . . H3 H 0.5058 0.8986 0.3432 0.027 Uiso 1 1 calc R . . C4 C 0.5297(5) 0.9398(5) 0.4819(12) 0.031(4) Uani 1 1 d . . . C5 C 0.5213(5) 0.9300(5) 0.5939(13) 0.034(4) Uani 1 1 d . . . H5 H 0.5396 0.9587 0.6411 0.041 Uiso 1 1 calc R . . C6 C 0.4886(5) 0.8819(6) 0.6353(11) 0.032(4) Uani 1 1 d . . . H6 H 0.4827 0.8781 0.7095 0.038 Uiso 1 1 calc R . . C7 C 0.5630(5) 0.9914(5) 0.4435(14) 0.034(4) Uani 1 1 d . . . C8 C 0.5551(5) 1.0070(5) 0.3407(13) 0.031(4) Uani 1 1 d . . . C9 C 0.5073(5) 0.9850(5) 0.2858(12) 0.028(3) Uani 1 1 d . . . H9 H 0.4776 0.9558 0.3165 0.033 Uiso 1 1 calc R . . C10 C 0.5011(6) 1.0032(6) 0.1909(15) 0.047(5) Uani 1 1 d . . . H10 H 0.4680 0.9871 0.1561 0.056 Uiso 1 1 calc R . . C11 C 0.5456(6) 1.0470(7) 0.1459(14) 0.047(5) Uani 1 1 d . . . C12 C 0.5939(6) 1.0699(7) 0.1986(16) 0.051(5) Uani 1 1 d . . . H12 H 0.6239 1.0989 0.1681 0.062 Uiso 1 1 calc R . . C13 C 0.5978(6) 1.0507(6) 0.2927(16) 0.045(5) Uani 1 1 d . . . H13 H 0.6307 1.0673 0.3281 0.053 Uiso 1 1 calc R . . C14 C 0.6035(6) 1.0268(6) 0.5128(16) 0.048(5) Uani 1 1 d . . . C15 C 0.6131(6) 1.0789(5) 0.5302(13) 0.034(4) Uani 1 1 d . . . H15 H 0.5946 1.0912 0.4883 0.041 Uiso 1 1 calc R . . C16 C 0.6472(5) 1.1113(7) 0.6035(13) 0.040(4) Uani 1 1 d . . . H16 H 0.6520 1.1453 0.6142 0.048 Uiso 1 1 calc R . . C17 C 0.6762(6) 1.0935(7) 0.6648(16) 0.053(6) Uani 1 1 d . . . C18 C 0.6694(7) 1.0451(8) 0.647(2) 0.076(7) Uani 1 1 d . . . H18 H 0.6894 1.0335 0.6853 0.091 Uiso 1 1 calc R . . C19 C 0.6337(7) 1.0127(7) 0.5727(19) 0.063(6) Uani 1 1 d . . . H19 H 0.6296 0.9788 0.5623 0.076 Uiso 1 1 calc R . . O9 O 0.3333 0.6667 0.6667 0.065(9) Uiso 1 6 d S . . 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 W1 0.0441(3) 0.0136(2) 0.0357(3) -0.0020(2) -0.0070(3) 0.0137(2) W2 0.0375(3) 0.0362(3) 0.0250(3) -0.0144(2) 0.0049(2) 0.0178(2) Zn1 0.0239(11) 0.0239(11) 0.0203(18) 0.000 0.000 0.0120(6) O1 0.060(6) 0.020(4) 0.055(7) -0.002(4) -0.026(5) 0.016(4) O2 0.047(5) 0.044(5) 0.036(6) -0.022(5) 0.013(5) 0.015(4) O7 0.012(8) 0.012(8) 0.016(13) 0.000 0.000 0.006(4) O8 0.017(7) 0.006(6) 0.020(9) 0.006(6) 0.004(7) -0.001(6) N1 0.061(8) 0.033(6) 0.026(7) 0.012(5) 0.003(6) 0.010(6) N2 0.046(8) 0.133(13) 0.075(11) 0.070(10) 0.014(8) 0.040(8) N3 0.043(7) 0.072(9) 0.090(12) -0.034(9) -0.027(8) 0.029(7) C1 0.045(7) 0.035(6) 0.032(8) -0.004(6) 0.004(6) 0.028(5) C2 0.026(5) 0.028(6) 0.023(7) -0.008(5) -0.005(5) 0.013(5) C3 0.027(5) 0.020(5) 0.021(6) 0.008(5) 0.005(5) 0.014(4) C4 0.037(6) 0.026(6) 0.036(8) 0.007(5) -0.005(6) 0.020(5) C5 0.040(6) 0.030(6) 0.040(9) -0.005(6) -0.003(6) 0.023(5) C6 0.047(7) 0.042(7) 0.013(6) -0.012(5) -0.008(5) 0.028(5) C7 0.018(6) 0.020(6) 0.058(10) 0.011(6) 0.002(6) 0.005(5) C8 0.020(5) 0.024(6) 0.051(9) 0.007(6) 0.014(6) 0.011(5) C9 0.028(5) 0.022(5) 0.038(8) 0.006(5) 0.006(6) 0.016(4) C10 0.031(6) 0.047(8) 0.067(11) 0.022(8) 0.016(7) 0.023(6) C11 0.049(8) 0.050(8) 0.043(9) 0.019(7) 0.009(7) 0.026(7) C12 0.035(7) 0.059(9) 0.063(11) 0.022(8) 0.015(8) 0.025(7) C13 0.028(7) 0.027(7) 0.073(12) -0.002(8) 0.008(8) 0.010(6) C14 0.046(7) 0.035(7) 0.068(12) -0.007(8) -0.017(8) 0.024(6) C15 0.029(6) 0.022(6) 0.042(8) -0.006(6) -0.016(6) 0.005(5) C16 0.016(6) 0.043(8) 0.046(9) -0.001(7) 0.016(6) 0.004(6) C17 0.024(7) 0.045(10) 0.064(12) -0.005(9) 0.007(8) -0.002(7) C18 0.047(8) 0.054(10) 0.129(19) -0.016(11) -0.048(11) 0.026(7) C19 0.046(8) 0.028(7) 0.113(16) -0.014(9) -0.041(10) 0.017(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 W1 O1 1.686(10) . ? W1 O3B 1.800(19) . ? W1 O5B 1.823(17) . ? W1 O4B 1.825(17) . ? W1 O3B 1.84(2) 15 ? W1 O5A 2.050(17) . ? W1 O3A 2.069(18) . ? W1 O4A 2.076(16) . ? W1 O3A 2.097(19) 15 ? W1 O8 2.220(18) . ? W1 O8 2.256(17) 15 ? W2 O2 1.702(11) . ? W2 O4B 1.795(18) 15 ? W2 O5B 1.804(16) . ? W2 O6B 1.81(2) . ? W2 O6B 1.83(2) 2_665 ? W2 O5A 2.038(16) . ? W2 O4A 2.061(17) 15 ? W2 O6A 2.081(19) . ? W2 O6A 2.08(2) 2_665 ? W2 O7 2.234(12) . ? W2 O8 2.241(17) 15 ? Zn1 O7 1.86(3) 13_565 ? Zn1 O7 1.86(3) . ? Zn1 O8 1.886(14) 14_455 ? Zn1 O8 1.886(14) 13_565 ? Zn1 O8 1.886(14) 2_665 ? Zn1 O8 1.886(14) . ? Zn1 O8 1.886(14) 3_565 ? Zn1 O8 1.886(14) 15 ? O3A W1 2.097(19) 14_455 ? O4A W2 2.061(17) 14_455 ? O6A W2 2.08(2) 3_565 ? O3B O8 1.81(2) . ? O3B W1 1.84(2) 14_455 ? O4B W2 1.795(18) 14_455 ? O6B W2 1.83(2) 3_565 ? O7 W2 2.234(12) 2_665 ? O7 W2 2.234(12) 3_565 ? O8 W2 2.241(17) 14_455 ? O8 W1 2.256(17) 14_455 ? N1 C1 1.276(19) . ? N1 H1A 0.8800 . ? N1 H1B 0.8800 . ? N2 C11 1.39(2) . ? N2 H2A 0.8800 . ? N2 H2B 0.8800 . ? N3 C17 1.40(2) . ? N3 H3A 0.8800 . ? N3 H3B 0.8800 . ? C1 C2 1.42(2) . ? C1 C6 1.419(19) . ? C2 C3 1.378(17) . ? C2 H2 0.9500 . ? C3 C4 1.418(19) . ? C3 H3 0.9500 . ? C4 C7 1.417(18) . ? C4 C5 1.44(2) . ? C5 C6 1.357(19) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C14 1.43(2) . ? C7 C8 1.44(2) . ? C8 C9 1.402(19) . ? C8 C13 1.409(19) . ? C9 C10 1.36(2) . ? C9 H9 0.9500 . ? C10 C11 1.42(2) . ? C10 H10 0.9500 . ? C11 C12 1.40(2) . ? C12 C13 1.35(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C19 1.38(3) . ? C14 C15 1.43(2) . ? C15 C16 1.35(2) . ? C15 H15 0.9500 . ? C16 C17 1.43(3) . ? C16 H16 0.9500 . ? C17 C18 1.35(3) . ? C18 C19 1.37(3) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 W1 O3B 111.2(7) . . ? O1 W1 O5B 112.0(7) . . ? O3B W1 O5B 75.9(8) . . ? O1 W1 O4B 111.4(7) . . ? O3B W1 O4B 90.6(8) . . ? O5B W1 O4B 136.5(7) . . ? O1 W1 O3B 109.7(6) . 15 ? O3B W1 O3B 139.0(10) . 15 ? O5B W1 O3B 89.2(7) . 15 ? O4B W1 O3B 74.2(7) . 15 ? O1 W1 O5A 90.3(6) . . ? O3B W1 O5A 90.5(8) . . ? O5B W1 O5A 23.0(7) . . ? O4B W1 O5A 156.1(6) . . ? O3B W1 O5A 89.5(7) 15 . ? O1 W1 O3A 88.6(6) . . ? O3B W1 O3A 23.6(7) . . ? O5B W1 O3A 90.3(7) . . ? O4B W1 O3A 92.9(7) . . ? O3B W1 O3A 160.4(7) 15 . ? O5A W1 O3A 97.6(7) . . ? O1 W1 O4A 87.8(6) . . ? O3B W1 O4A 91.3(7) . . ? O5B W1 O4A 159.2(8) . . ? O4B W1 O4A 25.2(6) . . ? O3B W1 O4A 90.0(7) 15 . ? O5A W1 O4A 177.7(7) . . ? O3A W1 O4A 83.6(7) . . ? O1 W1 O3A 87.5(6) . 15 ? O3B W1 O3A 160.1(7) . 15 ? O5B W1 O3A 91.2(7) . 15 ? O4B W1 O3A 88.5(7) . 15 ? O3B W1 O3A 23.3(6) 15 15 ? O5A W1 O3A 82.5(7) . 15 ? O3A W1 O3A 176.1(7) . 15 ? O4A W1 O3A 96.2(7) . 15 ? O1 W1 O8 151.7(6) . . ? O3B W1 O8 52.4(7) . . ? O5B W1 O8 87.7(7) . . ? O4B W1 O8 53.2(7) . . ? O3B W1 O8 89.7(6) 15 . ? O5A W1 O8 110.7(7) . . ? O3A W1 O8 70.7(6) . . ? O4A W1 O8 71.5(6) . . ? O3A W1 O8 113.0(6) 15 . ? O1 W1 O8 150.9(6) . 15 ? O3B W1 O8 90.7(7) . 15 ? O5B W1 O8 53.5(7) . 15 ? O4B W1 O8 86.3(6) . 15 ? O3B W1 O8 51.4(7) 15 15 ? O5A W1 O8 69.9(6) . 15 ? O3A W1 O8 114.3(6) . 15 ? O4A W1 O8 111.4(6) . 15 ? O3A W1 O8 69.5(6) 15 15 ? O8 W1 O8 57.2(7) . 15 ? O2 W2 O4B 110.8(7) . 15 ? O2 W2 O5B 110.8(7) . . ? O4B W2 O5B 93.2(8) 15 . ? O2 W2 O6B 110.7(7) . . ? O4B W2 O6B 138.4(8) 15 . ? O5B W2 O6B 73.1(8) . . ? O2 W2 O6B 110.2(7) . 2_665 ? O4B W2 O6B 72.9(7) 15 2_665 ? O5B W2 O6B 139.0(8) . 2_665 ? O6B W2 O6B 91.8(10) . 2_665 ? O2 W2 O5A 89.1(6) . . ? O4B W2 O5A 93.8(7) 15 . ? O5B W2 O5A 23.1(7) . . ? O6B W2 O5A 87.9(8) . . ? O6B W2 O5A 159.3(8) 2_665 . ? O2 W2 O4A 87.1(6) . 15 ? O4B W2 O4A 25.3(6) 15 15 ? O5B W2 O4A 93.8(8) . 15 ? O6B W2 O4A 160.6(8) . 15 ? O6B W2 O4A 88.9(7) 2_665 15 ? O5A W2 O4A 84.6(7) . 15 ? O2 W2 O6A 87.5(7) . . ? O4B W2 O6A 159.2(7) 15 . ? O5B W2 O6A 89.1(7) . . ? O6B W2 O6A 24.8(7) . . ? O6B W2 O6A 92.0(7) 2_665 . ? O5A W2 O6A 96.3(7) . . ? O4A W2 O6A 174.5(7) 15 . ? O2 W2 O6A 87.0(6) . 2_665 ? O4B W2 O6A 89.0(7) 15 2_665 ? O5B W2 O6A 159.8(8) . 2_665 ? O6B W2 O6A 92.1(7) . 2_665 ? O6B W2 O6A 24.9(7) 2_665 2_665 ? O5A W2 O6A 175.8(7) . 2_665 ? O4A W2 O6A 96.6(6) 15 2_665 ? O6A W2 O6A 82.0(9) . 2_665 ? O2 W2 O7 150.0(8) . . ? O4B W2 O7 88.9(6) 15 . ? O5B W2 O7 89.5(8) . . ? O6B W2 O7 53.0(6) . . ? O6B W2 O7 52.8(6) 2_665 . ? O5A W2 O7 112.6(7) . . ? O4A W2 O7 114.2(6) 15 . ? O6A W2 O7 70.5(7) . . ? O6A W2 O7 70.5(7) 2_665 . ? O2 W2 O8 151.1(6) . 15 ? O4B W2 O8 53.0(7) 15 15 ? O5B W2 O8 53.9(7) . 15 ? O6B W2 O8 89.3(7) . 15 ? O6B W2 O8 88.9(7) 2_665 15 ? O5A W2 O8 70.4(6) . 15 ? O4A W2 O8 71.3(6) 15 15 ? O6A W2 O8 114.1(7) . 15 ? O6A W2 O8 113.8(7) 2_665 15 ? O7 W2 O8 58.8(7) . 15 ? O7 Zn1 O7 179.996(6) 13_565 . ? O7 Zn1 O8 108.2(5) 13_565 14_455 ? O7 Zn1 O8 71.8(5) . 14_455 ? O7 Zn1 O8 108.2(5) 13_565 13_565 ? O7 Zn1 O8 71.8(5) . 13_565 ? O8 Zn1 O8 110.7(5) 14_455 13_565 ? O7 Zn1 O8 71.8(5) 13_565 2_665 ? O7 Zn1 O8 108.2(5) . 2_665 ? O8 Zn1 O8 179.997(1) 14_455 2_665 ? O8 Zn1 O8 69.3(5) 13_565 2_665 ? O7 Zn1 O8 71.8(5) 13_565 . ? O7 Zn1 O8 108.2(5) . . ? O8 Zn1 O8 69.3(5) 14_455 . ? O8 Zn1 O8 179.996(3) 13_565 . ? O8 Zn1 O8 110.7(5) 2_665 . ? O7 Zn1 O8 71.8(5) 13_565 3_565 ? O7 Zn1 O8 108.2(5) . 3_565 ? O8 Zn1 O8 69.3(5) 14_455 3_565 ? O8 Zn1 O8 69.3(5) 13_565 3_565 ? O8 Zn1 O8 110.7(5) 2_665 3_565 ? O8 Zn1 O8 110.7(5) . 3_565 ? O7 Zn1 O8 108.2(5) 13_565 15 ? O7 Zn1 O8 71.8(5) . 15 ? O8 Zn1 O8 110.7(5) 14_455 15 ? O8 Zn1 O8 110.7(5) 13_565 15 ? O8 Zn1 O8 69.3(5) 2_665 15 ? O8 Zn1 O8 69.3(5) . 15 ? O8 Zn1 O8 180.0(10) 3_565 15 ? W1 O3A W1 115.1(7) . 14_455 ? W2 O4A W1 114.0(8) 14_455 . ? W2 O5A W1 116.9(8) . . ? W2 O6A W2 114.3(8) . 3_565 ? W1 O3B O8 75.8(9) . . ? W1 O3B W1 149.9(10) . 14_455 ? O8 O3B W1 76.2(9) . 14_455 ? W2 O4B W1 146.7(11) 14_455 . ? W2 O5B W1 147.6(10) . . ? W2 O6B W2 147.4(10) . 3_565 ? Zn1 O7 W2 115.3(6) . . ? Zn1 O7 W2 115.3(6) . 2_665 ? W2 O7 W2 103.0(8) . 2_665 ? Zn1 O7 W2 115.3(6) . 3_565 ? W2 O7 W2 103.0(8) . 3_565 ? W2 O7 W2 103.0(8) 2_665 3_565 ? O3B O8 Zn1 129.5(11) . . ? O3B O8 W1 51.8(8) . . ? Zn1 O8 W1 117.6(8) . . ? O3B O8 W2 116.5(9) . 14_455 ? Zn1 O8 W2 114.0(7) . 14_455 ? W1 O8 W2 102.1(7) . 14_455 ? O3B O8 W1 52.4(7) . 14_455 ? Zn1 O8 W1 115.9(8) . 14_455 ? W1 O8 W1 103.5(6) . 14_455 ? W2 O8 W1 101.5(6) 14_455 14_455 ? C1 N1 H1A 120.0 . . ? C1 N1 H1B 120.0 . . ? H1A N1 H1B 120.0 . . ? C11 N2 H2A 120.0 . . ? C11 N2 H2B 120.0 . . ? H2A N2 H2B 120.0 . . ? C17 N3 H3A 120.0 . . ? C17 N3 H3B 120.0 . . ? H3A N3 H3B 120.0 . . ? N1 C1 C2 122.5(13) . . ? N1 C1 C6 119.3(14) . . ? C2 C1 C6 118.2(12) . . ? C3 C2 C1 120.0(12) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 123.5(13) . . ? C2 C3 H3 118.3 . . ? C4 C3 H3 118.3 . . ? C7 C4 C3 125.1(14) . . ? C7 C4 C5 120.5(13) . . ? C3 C4 C5 114.4(11) . . ? C6 C5 C4 123.3(13) . . ? C6 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? C5 C6 C1 120.4(13) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C4 C7 C14 116.7(15) . . ? C4 C7 C8 121.0(13) . . ? C14 C7 C8 122.2(13) . . ? C9 C8 C13 116.0(15) . . ? C9 C8 C7 125.9(12) . . ? C13 C8 C7 117.9(13) . . ? C10 C9 C8 123.8(12) . . ? C10 C9 H9 118.1 . . ? C8 C9 H9 118.1 . . ? C9 C10 C11 117.7(15) . . ? C9 C10 H10 121.1 . . ? C11 C10 H10 121.1 . . ? N2 C11 C12 120.3(15) . . ? N2 C11 C10 119.7(16) . . ? C12 C11 C10 120.0(16) . . ? C13 C12 C11 119.8(15) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C8 122.7(15) . . ? C12 C13 H13 118.7 . . ? C8 C13 H13 118.7 . . ? C19 C14 C7 123.1(16) . . ? C19 C14 C15 115.3(15) . . ? C7 C14 C15 121.5(16) . . ? C16 C15 C14 122.8(17) . . ? C16 C15 H15 118.6 . . ? C14 C15 H15 118.6 . . ? C15 C16 C17 118.9(17) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C18 C17 N3 121(2) . . ? C18 C17 C16 119.3(17) . . ? N3 C17 C16 119.5(18) . . ? C17 C18 C19 120(2) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C18 C19 C14 123.2(19) . . ? C18 C19 H19 118.4 . . ? C14 C19 H19 118.4 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.827 _refine_diff_density_min -2.321 _refine_diff_density_rms 0.292 #===END