Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author ; Sebastien Floquet Institut Lavoisier de Versailles, UMR 8180 Universite de Versailles Saint-Quentin-en-Yvelines 45 Avenue des Etats Unis 78035 Versailles Cedex France ; _publ_contact_author_phone '(33) 1 39 25 43 83 ' _publ_contact_author_fax '(33) 1 39 25 43 81' _publ_contact_author_email sebastien.floquet@chimie.uvsq.fr _publ_section_title ; Host-Guest adaptability and dynamics within oxothiomolybdenum wheels: Structures, studies in solution and DFT calculations ; # the loop structure below should contain the names and addresses of all # authors, in the required order of publication. repeat as necessary. loop_ _publ_author_name _publ_author_address J.-F.Lemonnier ; Institut Lavoisier de Versailles, UMR 8180 Universite de Versailles Saint-Quentin-en-Yvelines 45 Avenue des Etats Unis 78035 Versailles Cedex France ; S.Floquet ; Institut Lavoisier de Versailles, UMR 8180 Universite de Versailles Saint-Quentin-en-Yvelines 45 Avenue des Etats Unis 78035 Versailles Cedex France ; A.Kachmar ; Laboratoire de Chimie Quantique, Institut de chimie-UMR 7177, CNRS-ULP 4 rue Blaise Pascal 67000 Strasbourg France ; M.-M.Rohmer ; Laboratoire de Chimie Quantique, Institut de chimie-UMR 7177, CNRS-ULP 4 rue Blaise Pascal 67000 Strasbourg France ; M.Benard ; Laboratoire de Chimie Quantique, Institut de chimie-UMR 7177, CNRS-ULP 4 rue Blaise Pascal 67000 Strasbourg France ; ; J.Marrot ; ; Institut Lavoisier de Versailles, UMR 8180 Universite de Versailles Saint-Quentin-en-Yvelines 45 Avenue des Etats Unis 78035 Versailles Cedex France ; E.Terazzi ; Department of Inorganic, Analytical and Applied Chemistry University of Geneva 30 quai E. Ansermet, CH-1211 Geneva 4 Switzerland ; C.Piguet ; Department of Inorganic, Analytical and Applied Chemistry University of Geneva 30 quai E. Ansermet, CH-1211 Geneva 4 Switzerland ; E.Cadot ; Institut Lavoisier de Versailles, UMR 8180 Universite de Versailles Saint-Quentin-en-Yvelines 45 Avenue des Etats Unis 78035 Versailles Cedex France ; #==================================================================== # 4. text _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; sheldrick, g.m. (1993). shelxl-93. program for crystal structure determination. univ. of g\"ottingen, federal republic of germany. sheldrick, g.m. (1997). shelxs-86. program for the solution of crystal structures. univ. of g\"ottingen, federal republic of germany. ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; _publ_contact_author_name 'Sebastien Floquet' #==================================================================== data_Mo12Adip _database_code_depnum_ccdc_archive 'CCDC 640033' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H104 Mo12 N2 O58 S12' _chemical_formula_weight 2764.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 24.7548(14) _cell_length_b 11.3210(6) _cell_length_c 30.2286(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8471.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7170 _cell_measurement_theta_min 2.09 _cell_measurement_theta_max 38.89 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.168 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5448 _exptl_absorpt_coefficient_mu 2.103 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5711 _exptl_absorpt_correction_T_max 0.9206 _exptl_absorpt_process_details 'SADABS (Sheldrick, V2.10)' _exptl_special_details ; 'Blessing, Acta Cryst. (1995) A51, 33-38' ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 512x512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 81779 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 30.00 _reflns_number_total 12926 _reflns_number_gt 11026 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+33.9757P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12926 _refine_ls_number_parameters 518 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0549 _refine_ls_R_factor_gt 0.0427 _refine_ls_wR_factor_ref 0.1341 _refine_ls_wR_factor_gt 0.1191 _refine_ls_goodness_of_fit_ref 1.209 _refine_ls_restrained_S_all 1.209 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.353935(19) 0.7500 0.656654(16) 0.01537(10) Uani 1 2 d S . . Mo2 Mo 0.26296(2) 0.7500 0.711339(16) 0.01713(11) Uani 1 2 d S . . Mo3 Mo 0.13538(2) 0.7500 0.688569(17) 0.01951(11) Uani 1 2 d S . . Mo4 Mo 0.067135(19) 0.7500 0.614219(17) 0.01659(11) Uani 1 2 d S . . Mo5 Mo 0.026047(19) 0.7500 0.510973(16) 0.01435(10) Uani 1 2 d S . . Mo6 Mo 0.022487(19) 0.7500 0.418210(16) 0.01445(10) Uani 1 2 d S . . Mo7 Mo 0.101488(19) 0.7500 0.328184(17) 0.01534(10) Uani 1 2 d S . . Mo8 Mo 0.20502(2) 0.7500 0.290664(17) 0.01650(11) Uani 1 2 d S . . Mo9 Mo 0.33588(2) 0.7500 0.317573(18) 0.02099(12) Uani 1 2 d S . . Mo10 Mo 0.42161(2) 0.7500 0.379302(18) 0.02234(12) Uani 1 2 d S . . Mo11 Mo 0.47228(2) 0.7500 0.480377(17) 0.01760(11) Uani 1 2 d S . . Mo12 Mo 0.44007(2) 0.7500 0.570693(17) 0.01701(11) Uani 1 2 d S . . S1 S 0.30612(4) 0.91380(10) 0.68112(4) 0.0201(2) Uani 1 1 d . . . S2 S 0.10952(4) 0.91071(11) 0.64558(4) 0.0211(2) Uani 1 1 d . . . S3 S 0.04003(4) 0.90831(9) 0.46430(3) 0.01781(19) Uani 1 1 d . . . S4 S 0.15411(4) 0.58607(10) 0.31126(4) 0.0186(2) Uani 1 1 d . . . S5 S 0.36647(5) 0.90838(11) 0.35985(4) 0.0254(2) Uani 1 1 d . . . S6 S 0.44494(4) 0.59056(10) 0.52303(3) 0.0191(2) Uani 1 1 d . . . O1 O 0.40648(18) 0.7500 0.69252(16) 0.0235(9) Uani 1 2 d S . . O2 O 0.28740(18) 0.7500 0.76401(15) 0.0222(9) Uani 1 2 d S . . O3 O 0.08916(19) 0.7500 0.72984(16) 0.0284(11) Uani 1 2 d S . . O4 O 0.00343(18) 0.7500 0.63511(16) 0.0239(10) Uani 1 2 d S . . O5 O -0.03965(18) 0.7500 0.52425(16) 0.0219(9) Uani 1 2 d S . . O6 O -0.04594(18) 0.7500 0.41050(15) 0.0199(9) Uani 1 2 d S . . O7 O 0.05864(18) 0.7500 0.28455(15) 0.0213(9) Uani 1 2 d S . . O8 O 0.1961(2) 0.7500 0.23491(15) 0.0262(10) Uani 1 2 d S . . O9 O 0.37600(19) 0.7500 0.27309(16) 0.0250(10) Uani 1 2 d S . . O10 O 0.4703(2) 0.7500 0.34054(16) 0.0308(11) Uani 1 2 d S . . O11 O 0.54042(18) 0.7500 0.48704(15) 0.0226(9) Uani 1 2 d S . . O12 O 0.49847(19) 0.7500 0.59870(16) 0.0241(9) Uani 1 2 d S . . O13 O 0.38905(13) 0.6444(3) 0.60715(11) 0.0216(6) Uani 1 1 d . . . O14 O 0.19370(12) 0.6441(3) 0.71817(10) 0.0222(7) Uani 1 1 d . . . O15 O 0.06393(13) 0.8535(3) 0.55809(10) 0.0191(6) Uani 1 1 d . . . O16 O 0.05437(12) 0.8560(3) 0.37002(10) 0.0186(6) Uani 1 1 d . . . O17 O 0.27463(12) 0.8580(3) 0.29361(11) 0.0206(6) Uani 1 1 d . . . O18 O 0.46386(14) 0.8587(3) 0.42483(11) 0.0251(7) Uani 1 1 d . . . O19 O 0.28914(18) 0.7500 0.60047(14) 0.0216(9) Uani 1 2 d S . . O20 O 0.21651(17) 0.7500 0.64412(14) 0.0173(8) Uani 1 2 d S . . O21 O 0.14942(17) 0.7500 0.39352(14) 0.0172(8) Uani 1 2 d S . . O22 O 0.23171(17) 0.7500 0.36258(14) 0.0173(8) Uani 1 2 d S . . O23 O 0.3757(2) 0.7500 0.45187(17) 0.0271(10) Uani 1 2 d S . . C1 C 0.2384(2) 0.7500 0.6059(2) 0.0188(11) Uani 1 2 d S . . C2 C 0.2018(3) 0.7500 0.5661(2) 0.0314(17) Uani 1 2 d S . . H2A H 0.1782 0.8205 0.5676 0.038 Uiso 0.50 1 calc PR . . H2B H 0.1782 0.6795 0.5676 0.038 Uiso 0.50 1 calc PR . . C3 C 0.2302(3) 0.7500 0.5220(2) 0.0267(14) Uani 1 2 d S . . H3A H 0.2538 0.6795 0.5207 0.032 Uiso 0.50 1 calc PR . . H3B H 0.2538 0.8205 0.5207 0.032 Uiso 0.50 1 calc PR . . C4 C 0.1945(3) 0.7500 0.4816(2) 0.0282(15) Uani 1 2 d S . . H4A H 0.1710 0.6792 0.4820 0.034 Uiso 0.50 1 calc PR . . H4B H 0.1710 0.8208 0.4820 0.034 Uiso 0.50 1 calc PR . . C5 C 0.2278(3) 0.7500 0.4404(2) 0.0313(16) Uani 1 2 d S . . H5A H 0.2516 0.6797 0.4415 0.038 Uiso 0.50 1 calc PR . . H5B H 0.2516 0.8203 0.4415 0.038 Uiso 0.50 1 calc PR . . C6 C 0.2003(2) 0.7500 0.3957(2) 0.0175(11) Uani 1 2 d S . . N7 N 0.00752(16) 0.4885(4) 0.23225(14) 0.0237(8) Uani 1 1 d . . . C8 C -0.0189(2) 0.4136(5) 0.19683(18) 0.0291(10) Uani 1 1 d . . . H8A H 0.0076 0.3573 0.1851 0.044 Uiso 1 1 calc R . . H8B H -0.0318 0.4646 0.1729 0.044 Uiso 1 1 calc R . . H8C H -0.0494 0.3703 0.2096 0.044 Uiso 1 1 calc R . . C9 C 0.0289(2) 0.4121(5) 0.26865(18) 0.0313(11) Uani 1 1 d . . . H9A H -0.0007 0.3662 0.2815 0.047 Uiso 1 1 calc R . . H9B H 0.0453 0.4618 0.2916 0.047 Uiso 1 1 calc R . . H9C H 0.0563 0.3582 0.2567 0.047 Uiso 1 1 calc R . . C10 C -0.0343(2) 0.5713(5) 0.2503(2) 0.0358(13) Uani 1 1 d . . . H10A H -0.0475 0.6226 0.2266 0.054 Uiso 1 1 calc R . . H10B H -0.0182 0.6197 0.2738 0.054 Uiso 1 1 calc R . . H10C H -0.0645 0.5256 0.2625 0.054 Uiso 1 1 calc R . . C11 C 0.0532(2) 0.5548(5) 0.2121(2) 0.0319(11) Uani 1 1 d . . . H11A H 0.0802 0.4989 0.2011 0.048 Uiso 1 1 calc R . . H11B H 0.0697 0.6060 0.2345 0.048 Uiso 1 1 calc R . . H11C H 0.0398 0.6031 0.1876 0.048 Uiso 1 1 calc R . . O1W O 0.08269(13) 0.4152(3) 0.38395(11) 0.0223(6) Uani 1 1 d . . . O2W O 0.42063(14) 0.4277(3) 0.44027(12) 0.0267(7) Uani 1 1 d . . . O3W O 0.14727(14) 0.3750(3) 0.45893(13) 0.0277(7) Uani 1 1 d . . . O4W O -0.11236(14) 0.9360(3) 0.45357(13) 0.0290(7) Uani 1 1 d . . . O5W O 0.3849(3) 0.2500 0.3871(2) 0.0388(14) Uani 1 2 d S . . O6W O 0.32798(14) 0.5416(4) 0.47060(13) 0.0324(8) Uani 1 1 d . . . O7W O 0.75928(16) 0.4253(3) 0.17103(13) 0.0306(8) Uani 1 1 d . . . O8W O 0.8315(2) 0.2500 0.18871(17) 0.0335(12) Uani 1 2 d S . . O9W O 0.6412(3) 0.7500 0.3475(2) 0.0418(14) Uani 1 2 d S . . O10W O 0.3917(2) 0.7500 0.1766(2) 0.0428(15) Uani 1 2 d S . . O11W O 0.30621(16) 0.5886(4) 0.20012(14) 0.0365(9) Uani 1 1 d . . . O12W O 0.24465(16) 0.4455(4) 0.42167(15) 0.0435(11) Uani 1 1 d . . . O13W O 0.8004(3) 0.2500 0.0528(2) 0.0511(17) Uani 1 2 d S . . O14W O 0.1265(3) 0.2500 0.3252(2) 0.0511(18) Uani 1 2 d S . . O15W O 0.8452(3) 0.2500 0.9665(2) 0.0486(16) Uani 1 2 d S . . O16W O 0.0840(3) 0.9146(5) 0.10583(18) 0.0606(15) Uani 1 1 d . . . O17W O 0.8079(2) 0.0131(5) 0.94099(19) 0.0629(15) Uani 1 1 d . . . O18W O -0.2112(3) 0.9041(12) 0.4009(3) 0.100(4) Uani 0.75 1 d P . . O19W O -0.2494(6) 0.8005(16) 0.3690(6) 0.045(5) Uani 0.25 1 d P . . 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 0.0106(2) 0.0226(2) 0.0130(2) 0.000 0.00039(16) 0.000 Mo2 0.0099(2) 0.0301(3) 0.0114(2) 0.000 -0.00047(16) 0.000 Mo3 0.0101(2) 0.0356(3) 0.0128(2) 0.000 -0.00035(16) 0.000 Mo4 0.0095(2) 0.0268(3) 0.0135(2) 0.000 -0.00064(16) 0.000 Mo5 0.0100(2) 0.0190(2) 0.0141(2) 0.000 -0.00048(16) 0.000 Mo6 0.0100(2) 0.0186(2) 0.0148(2) 0.000 -0.00111(16) 0.000 Mo7 0.0112(2) 0.0210(2) 0.0139(2) 0.000 -0.00145(16) 0.000 Mo8 0.0131(2) 0.0233(3) 0.0131(2) 0.000 -0.00038(16) 0.000 Mo9 0.0188(2) 0.0290(3) 0.0151(2) 0.000 -0.00566(18) 0.000 Mo10 0.0200(2) 0.0323(3) 0.0148(2) 0.000 -0.00637(19) 0.000 Mo11 0.0114(2) 0.0285(3) 0.0129(2) 0.000 -0.00204(16) 0.000 Mo12 0.0126(2) 0.0237(3) 0.0147(2) 0.000 0.00208(17) 0.000 S1 0.0153(4) 0.0246(5) 0.0203(5) -0.0027(4) 0.0014(4) 0.0012(4) S2 0.0160(4) 0.0288(6) 0.0186(5) -0.0052(4) -0.0038(4) 0.0014(4) S3 0.0181(4) 0.0195(5) 0.0158(4) -0.0005(4) -0.0009(3) -0.0004(4) S4 0.0146(4) 0.0215(5) 0.0197(5) -0.0015(4) -0.0007(4) -0.0001(4) S5 0.0259(5) 0.0290(6) 0.0214(5) 0.0015(4) -0.0104(4) -0.0034(4) S6 0.0163(4) 0.0248(5) 0.0161(4) -0.0008(4) -0.0012(3) 0.0017(4) O1 0.0130(19) 0.034(3) 0.023(2) 0.000 -0.0007(17) 0.000 O2 0.0144(19) 0.035(3) 0.017(2) 0.000 -0.0026(16) 0.000 O3 0.015(2) 0.054(3) 0.016(2) 0.000 0.0013(17) 0.000 O4 0.0120(19) 0.040(3) 0.019(2) 0.000 0.0004(16) 0.000 O5 0.0138(19) 0.029(2) 0.023(2) 0.000 -0.0012(17) 0.000 O6 0.0143(19) 0.028(2) 0.017(2) 0.000 -0.0028(16) 0.000 O7 0.0147(19) 0.033(2) 0.016(2) 0.000 -0.0045(16) 0.000 O8 0.028(2) 0.036(3) 0.015(2) 0.000 -0.0031(18) 0.000 O9 0.016(2) 0.037(3) 0.022(2) 0.000 -0.0049(17) 0.000 O10 0.027(2) 0.049(3) 0.017(2) 0.000 -0.0053(19) 0.000 O11 0.0127(19) 0.036(3) 0.019(2) 0.000 0.0007(16) 0.000 O12 0.018(2) 0.037(3) 0.017(2) 0.000 -0.0012(17) 0.000 O13 0.0199(14) 0.0229(15) 0.0219(15) -0.0005(13) 0.0072(12) 0.0000(12) O14 0.0123(13) 0.0383(19) 0.0159(14) 0.0061(13) -0.0016(11) -0.0025(13) O15 0.0193(14) 0.0218(15) 0.0164(13) 0.0004(12) -0.0029(11) -0.0006(12) O16 0.0136(13) 0.0222(15) 0.0201(14) -0.0002(12) 0.0004(11) 0.0011(11) O17 0.0154(13) 0.0263(16) 0.0202(14) 0.0016(13) 0.0002(11) -0.0033(12) O18 0.0225(15) 0.0371(19) 0.0155(14) 0.0017(14) -0.0062(12) -0.0009(14) O19 0.0132(19) 0.039(3) 0.0126(19) 0.000 -0.0009(15) 0.000 O20 0.0126(18) 0.024(2) 0.0149(18) 0.000 -0.0018(15) 0.000 O21 0.0146(18) 0.020(2) 0.0170(19) 0.000 -0.0031(15) 0.000 O22 0.0142(18) 0.023(2) 0.0143(19) 0.000 -0.0024(15) 0.000 O23 0.020(2) 0.036(3) 0.025(2) 0.000 -0.0079(19) 0.000 C1 0.018(3) 0.025(3) 0.013(2) 0.000 0.001(2) 0.000 C2 0.011(3) 0.068(5) 0.014(3) 0.000 -0.003(2) 0.000 C3 0.018(3) 0.048(4) 0.014(3) 0.000 -0.001(2) 0.000 C4 0.016(3) 0.055(5) 0.014(3) 0.000 -0.003(2) 0.000 C5 0.023(3) 0.056(5) 0.014(3) 0.000 -0.004(2) 0.000 C6 0.019(3) 0.016(3) 0.018(3) 0.000 -0.002(2) 0.000 N7 0.0203(17) 0.0196(18) 0.031(2) -0.0048(16) 0.0021(15) 0.0001(14) C8 0.028(2) 0.030(3) 0.029(2) 0.000(2) -0.0076(19) -0.0021(19) C9 0.029(2) 0.037(3) 0.028(2) -0.006(2) -0.008(2) -0.002(2) C10 0.022(2) 0.028(2) 0.058(4) -0.009(3) 0.015(2) 0.0002(19) C11 0.026(2) 0.027(2) 0.043(3) -0.007(2) 0.012(2) -0.0021(19) O1W 0.0189(14) 0.0235(16) 0.0246(16) -0.0015(13) 0.0022(12) -0.0005(12) O2W 0.0208(15) 0.0313(18) 0.0281(17) -0.0018(15) -0.0072(13) 0.0033(13) O3W 0.0183(14) 0.0302(18) 0.0347(19) 0.0047(15) 0.0028(13) -0.0006(13) O4W 0.0246(16) 0.0289(18) 0.0336(19) -0.0001(15) 0.0086(14) -0.0005(14) O5W 0.037(3) 0.034(3) 0.045(3) 0.000 -0.021(3) 0.000 O6W 0.0205(16) 0.042(2) 0.0347(19) -0.0050(17) -0.0072(15) -0.0008(15) O7W 0.0306(18) 0.0267(18) 0.0345(19) 0.0013(15) 0.0124(15) -0.0020(15) O8W 0.042(3) 0.043(3) 0.016(2) 0.000 -0.001(2) 0.000 O9W 0.034(3) 0.060(4) 0.032(3) 0.000 0.013(2) 0.000 O10W 0.031(3) 0.070(4) 0.028(3) 0.000 0.008(2) 0.000 O11W 0.0281(18) 0.041(2) 0.040(2) -0.0082(18) 0.0094(17) -0.0080(16) O12W 0.0227(18) 0.067(3) 0.041(2) -0.007(2) 0.0017(16) -0.0145(19) O13W 0.044(4) 0.062(4) 0.047(4) 0.000 0.004(3) 0.000 O14W 0.055(4) 0.050(4) 0.049(4) 0.000 0.035(3) 0.000 O15W 0.031(3) 0.070(5) 0.045(4) 0.000 -0.001(3) 0.000 O16W 0.084(4) 0.052(3) 0.046(3) 0.003(2) -0.019(3) -0.003(3) O17W 0.067(4) 0.068(4) 0.053(3) -0.021(3) -0.013(3) 0.013(3) O18W 0.025(3) 0.215(12) 0.061(5) 0.025(7) 0.009(3) -0.008(5) O19W 0.018(6) 0.064(11) 0.053(10) 0.045(8) -0.005(6) -0.010(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.693(5) . ? Mo1 O13 2.103(3) . ? Mo1 O13 2.103(3) 7_575 ? Mo1 S1 2.3208(11) 7_575 ? Mo1 S1 2.3209(11) . ? Mo1 O19 2.336(4) . ? Mo1 Mo2 2.7936(7) . ? Mo2 O2 1.703(5) . ? Mo2 O14 2.102(3) . ? Mo2 O14 2.102(3) 7_575 ? Mo2 S1 2.3269(12) . ? Mo2 S1 2.3270(12) 7_575 ? Mo2 O20 2.335(4) . ? Mo3 O3 1.693(5) . ? Mo3 O14 2.079(3) 7_575 ? Mo3 O14 2.079(3) . ? Mo3 S2 2.3257(12) 7_575 ? Mo3 S2 2.3257(12) . ? Mo3 O20 2.416(4) . ? Mo3 Mo4 2.8116(7) . ? Mo4 O4 1.699(4) . ? Mo4 O15 2.063(3) . ? Mo4 O15 2.063(3) 7_575 ? Mo4 S2 2.3043(12) 7_575 ? Mo4 S2 2.3043(12) . ? Mo5 O5 1.675(4) . ? Mo5 O15 2.069(3) 7_575 ? Mo5 O15 2.069(3) . ? Mo5 S3 2.3071(11) . ? Mo5 S3 2.3071(11) 7_575 ? Mo5 Mo6 2.8055(7) . ? Mo6 O6 1.710(4) . ? Mo6 O16 2.046(3) . ? Mo6 O16 2.046(3) 7_575 ? Mo6 S3 2.3110(11) 7_575 ? Mo6 S3 2.3111(11) . ? Mo7 O7 1.693(4) . ? Mo7 O16 2.098(3) . ? Mo7 O16 2.098(3) 7_575 ? Mo7 O21 2.304(4) . ? Mo7 S4 2.3243(11) 7_575 ? Mo7 S4 2.3243(11) . ? Mo7 Mo8 2.8027(7) . ? Mo8 O8 1.700(5) . ? Mo8 O17 2.115(3) 7_575 ? Mo8 O17 2.115(3) . ? Mo8 O22 2.272(4) . ? Mo8 S4 2.3282(11) . ? Mo8 S4 2.3283(11) 7_575 ? Mo9 O9 1.672(5) . ? Mo9 O17 2.078(3) . ? Mo9 O17 2.078(3) 7_575 ? Mo9 S5 2.3284(12) 7_575 ? Mo9 S5 2.3285(12) . ? Mo9 Mo10 2.8259(7) . ? Mo10 O10 1.681(5) . ? Mo10 O18 2.122(3) 7_575 ? Mo10 O18 2.122(3) . ? Mo10 S5 2.3289(13) . ? Mo10 S5 2.3289(13) 7_575 ? Mo10 O23 2.471(5) . ? Mo11 O11 1.699(4) . ? Mo11 O18 2.092(3) . ? Mo11 O18 2.092(3) 7_575 ? Mo11 S6 2.3191(12) 7_575 ? Mo11 S6 2.3191(12) . ? Mo11 Mo12 2.8441(7) . ? Mo12 O12 1.675(5) . ? Mo12 O13 2.059(3) 7_575 ? Mo12 O13 2.059(3) . ? Mo12 S6 2.3127(11) . ? Mo12 S6 2.3128(12) 7_575 ? O19 C1 1.267(7) . ? O20 C1 1.277(7) . ? O21 C6 1.260(7) . ? O22 C6 1.268(8) . ? C1 C2 1.505(9) . ? C2 C3 1.506(9) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.508(9) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.496(9) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.513(9) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? N7 C11 1.486(6) . ? N7 C9 1.497(7) . ? N7 C10 1.499(6) . ? N7 C8 1.514(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? O18W O19W 1.79(2) . ? O19W O19W 1.14(4) 7_575 ? 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 O13 97.94(16) . . ? O1 Mo1 O13 97.94(16) . 7_575 ? O13 Mo1 O13 69.26(18) . 7_575 ? O1 Mo1 S1 100.83(10) . 7_575 ? O13 Mo1 S1 89.05(9) . 7_575 ? O13 Mo1 S1 153.06(10) 7_575 7_575 ? O1 Mo1 S1 100.82(10) . . ? O13 Mo1 S1 153.07(10) . . ? O13 Mo1 S1 89.05(9) 7_575 . ? S1 Mo1 S1 106.07(6) 7_575 . ? O1 Mo1 O19 173.2(2) . . ? O13 Mo1 O19 76.49(13) . . ? O13 Mo1 O19 76.49(13) 7_575 . ? S1 Mo1 O19 83.19(7) 7_575 . ? S1 Mo1 O19 83.19(7) . . ? O1 Mo1 Mo2 103.91(16) . . ? O13 Mo1 Mo2 138.95(9) . . ? O13 Mo1 Mo2 138.95(9) 7_575 . ? S1 Mo1 Mo2 53.15(3) 7_575 . ? S1 Mo1 Mo2 53.15(3) . . ? O19 Mo1 Mo2 82.92(11) . . ? O2 Mo2 O14 101.41(15) . . ? O2 Mo2 O14 101.41(15) . 7_575 ? O14 Mo2 O14 69.53(19) . 7_575 ? O2 Mo2 S1 101.77(9) . . ? O14 Mo2 S1 150.16(9) . . ? O14 Mo2 S1 87.63(10) 7_575 . ? O2 Mo2 S1 101.77(9) . 7_575 ? O14 Mo2 S1 87.63(10) . 7_575 ? O14 Mo2 S1 150.16(9) 7_575 7_575 ? S1 Mo2 S1 105.67(6) . 7_575 ? O2 Mo2 O20 171.30(19) . . ? O14 Mo2 O20 71.56(12) . . ? O14 Mo2 O20 71.56(12) 7_575 . ? S1 Mo2 O20 83.36(7) . . ? S1 Mo2 O20 83.36(7) 7_575 . ? O2 Mo2 Mo1 105.48(15) . . ? O14 Mo2 Mo1 135.69(10) . . ? O14 Mo2 Mo1 135.69(10) 7_575 . ? S1 Mo2 Mo1 52.95(3) . . ? S1 Mo2 Mo1 52.95(3) 7_575 . ? O20 Mo2 Mo1 83.23(11) . . ? O3 Mo3 O14 98.75(16) . 7_575 ? O3 Mo3 O14 98.76(16) . . ? O14 Mo3 O14 70.43(19) 7_575 . ? O3 Mo3 S2 103.04(10) . 7_575 ? O14 Mo3 S2 151.98(9) 7_575 7_575 ? O14 Mo3 S2 88.89(10) . 7_575 ? O3 Mo3 S2 103.04(10) . . ? O14 Mo3 S2 88.88(10) 7_575 . ? O14 Mo3 S2 151.98(9) . . ? S2 Mo3 S2 102.95(6) 7_575 . ? O3 Mo3 O20 166.32(19) . . ? O14 Mo3 O20 70.26(12) 7_575 . ? O14 Mo3 O20 70.26(12) . . ? S2 Mo3 O20 85.30(7) 7_575 . ? S2 Mo3 O20 85.30(7) . . ? O3 Mo3 Mo4 100.54(16) . . ? O14 Mo3 Mo4 139.58(10) 7_575 . ? O14 Mo3 Mo4 139.58(10) . . ? S2 Mo3 Mo4 52.26(3) 7_575 . ? S2 Mo3 Mo4 52.26(3) . . ? O20 Mo3 Mo4 93.15(10) . . ? O4 Mo4 O15 105.66(16) . . ? O4 Mo4 O15 105.66(16) . 7_575 ? O15 Mo4 O15 69.19(18) . 7_575 ? O4 Mo4 S2 105.65(10) . 7_575 ? O15 Mo4 S2 143.53(10) . 7_575 ? O15 Mo4 S2 84.70(9) 7_575 7_575 ? O4 Mo4 S2 105.65(10) . . ? O15 Mo4 S2 84.69(9) . . ? O15 Mo4 S2 143.53(10) 7_575 . ? S2 Mo4 S2 104.29(6) 7_575 . ? O4 Mo4 Mo3 105.11(16) . . ? O15 Mo4 Mo3 132.88(9) . . ? O15 Mo4 Mo3 132.88(9) 7_575 . ? S2 Mo4 Mo3 52.95(3) 7_575 . ? S2 Mo4 Mo3 52.95(3) . . ? O5 Mo5 O15 105.97(16) . 7_575 ? O5 Mo5 O15 105.97(16) . . ? O15 Mo5 O15 68.98(18) 7_575 . ? O5 Mo5 S3 106.99(10) . . ? O15 Mo5 S3 142.46(9) 7_575 . ? O15 Mo5 S3 85.02(9) . . ? O5 Mo5 S3 106.98(10) . 7_575 ? O15 Mo5 S3 85.02(9) 7_575 7_575 ? O15 Mo5 S3 142.46(9) . 7_575 ? S3 Mo5 S3 101.94(6) . 7_575 ? O5 Mo5 Mo6 102.06(16) . . ? O15 Mo5 Mo6 134.61(9) 7_575 . ? O15 Mo5 Mo6 134.61(9) . . ? S3 Mo5 Mo6 52.66(3) . . ? S3 Mo5 Mo6 52.66(3) 7_575 . ? O6 Mo6 O16 106.56(15) . . ? O6 Mo6 O16 106.56(15) . 7_575 ? O16 Mo6 O16 71.84(18) . 7_575 ? O6 Mo6 S3 105.56(9) . 7_575 ? O16 Mo6 S3 144.26(9) . 7_575 ? O16 Mo6 S3 84.36(9) 7_575 7_575 ? O6 Mo6 S3 105.56(10) . . ? O16 Mo6 S3 84.36(9) . . ? O16 Mo6 S3 144.26(9) 7_575 . ? S3 Mo6 S3 101.70(6) 7_575 . ? O6 Mo6 Mo5 99.64(15) . . ? O16 Mo6 Mo5 134.39(9) . . ? O16 Mo6 Mo5 134.40(9) 7_575 . ? S3 Mo6 Mo5 52.53(3) 7_575 . ? S3 Mo6 Mo5 52.53(3) . . ? O7 Mo7 O16 96.97(15) . . ? O7 Mo7 O16 96.97(15) . 7_575 ? O16 Mo7 O16 69.81(17) . 7_575 ? O7 Mo7 O21 172.19(19) . . ? O16 Mo7 O21 76.68(12) . . ? O16 Mo7 O21 76.68(12) 7_575 . ? O7 Mo7 S4 100.35(10) . 7_575 ? O16 Mo7 S4 89.28(9) . 7_575 ? O16 Mo7 S4 154.31(9) 7_575 7_575 ? O21 Mo7 S4 84.26(7) . 7_575 ? O7 Mo7 S4 100.35(10) . . ? O16 Mo7 S4 154.31(9) . . ? O16 Mo7 S4 89.28(9) 7_575 . ? O21 Mo7 S4 84.26(7) . . ? S4 Mo7 S4 105.97(6) 7_575 . ? O7 Mo7 Mo8 104.93(16) . . ? O16 Mo7 Mo8 138.80(9) . . ? O16 Mo7 Mo8 138.80(9) 7_575 . ? O21 Mo7 Mo8 82.87(11) . . ? S4 Mo7 Mo8 53.02(3) 7_575 . ? S4 Mo7 Mo8 53.02(3) . . ? O8 Mo8 O17 98.48(17) . 7_575 ? O8 Mo8 O17 98.49(17) . . ? O17 Mo8 O17 70.65(18) 7_575 . ? O8 Mo8 O22 170.6(2) . . ? O17 Mo8 O22 73.91(12) 7_575 . ? O17 Mo8 O22 73.90(12) . . ? O8 Mo8 S4 101.24(11) . . ? O17 Mo8 S4 88.22(9) 7_575 . ? O17 Mo8 S4 152.97(9) . . ? O22 Mo8 S4 84.35(7) . . ? O8 Mo8 S4 101.24(11) . 7_575 ? O17 Mo8 S4 152.97(9) 7_575 7_575 ? O17 Mo8 S4 88.22(9) . 7_575 ? O22 Mo8 S4 84.35(7) . 7_575 ? S4 Mo8 S4 105.71(6) . 7_575 ? O8 Mo8 Mo7 106.41(18) . . ? O17 Mo8 Mo7 136.72(9) 7_575 . ? O17 Mo8 Mo7 136.72(9) . . ? O22 Mo8 Mo7 83.04(11) . . ? S4 Mo8 Mo7 52.89(3) . . ? S4 Mo8 Mo7 52.89(3) 7_575 . ? O9 Mo9 O17 98.81(15) . . ? O9 Mo9 O17 98.80(15) . 7_575 ? O17 Mo9 O17 72.10(18) . 7_575 ? O9 Mo9 S5 104.37(10) . 7_575 ? O17 Mo9 S5 151.85(10) . 7_575 ? O17 Mo9 S5 88.59(9) 7_575 7_575 ? O9 Mo9 S5 104.37(10) . . ? O17 Mo9 S5 88.59(9) . . ? O17 Mo9 S5 151.85(10) 7_575 . ? S5 Mo9 S5 100.72(6) 7_575 . ? O9 Mo9 Mo10 94.87(16) . . ? O17 Mo9 Mo10 141.08(9) . . ? O17 Mo9 Mo10 141.08(9) 7_575 . ? S5 Mo9 Mo10 52.65(3) 7_575 . ? S5 Mo9 Mo10 52.65(3) . . ? O10 Mo10 O18 95.65(17) . 7_575 ? O10 Mo10 O18 95.65(17) . . ? O18 Mo10 O18 70.90(19) 7_575 . ? O10 Mo10 S5 104.15(11) . . ? O18 Mo10 S5 154.05(10) 7_575 . ? O18 Mo10 S5 90.35(10) . . ? O10 Mo10 S5 104.14(11) . 7_575 ? O18 Mo10 S5 90.35(10) 7_575 7_575 ? O18 Mo10 S5 154.05(10) . 7_575 ? S5 Mo10 S5 100.69(6) . 7_575 ? O10 Mo10 O23 161.6(2) . . ? O18 Mo10 O23 69.57(13) 7_575 . ? O18 Mo10 O23 69.57(13) . . ? S5 Mo10 O23 87.39(8) . . ? S5 Mo10 O23 87.40(8) 7_575 . ? O10 Mo10 Mo9 94.50(17) . . ? O18 Mo10 Mo9 142.98(10) 7_575 . ? O18 Mo10 Mo9 142.98(10) . . ? S5 Mo10 Mo9 52.64(3) . . ? S5 Mo10 Mo9 52.64(3) 7_575 . ? O23 Mo10 Mo9 103.93(11) . . ? O11 Mo11 O18 101.19(16) . . ? O11 Mo11 O18 101.19(16) . 7_575 ? O18 Mo11 O18 72.1(2) . 7_575 ? O11 Mo11 S6 102.94(10) . 7_575 ? O18 Mo11 S6 87.66(10) . 7_575 ? O18 Mo11 S6 151.02(10) 7_575 7_575 ? O11 Mo11 S6 102.94(10) . . ? O18 Mo11 S6 151.03(10) . . ? O18 Mo11 S6 87.66(10) 7_575 . ? S6 Mo11 S6 102.21(6) 7_575 . ? O11 Mo11 Mo12 99.48(16) . . ? O18 Mo11 Mo12 137.94(10) . . ? O18 Mo11 Mo12 137.94(10) 7_575 . ? S6 Mo11 Mo12 52.02(3) 7_575 . ? S6 Mo11 Mo12 52.02(3) . . ? O12 Mo12 O13 105.01(16) . 7_575 ? O12 Mo12 O13 105.01(16) . . ? O13 Mo12 O13 70.98(18) 7_575 . ? O12 Mo12 S6 105.66(10) . . ? O13 Mo12 S6 144.94(10) 7_575 . ? O13 Mo12 S6 84.97(10) . . ? O12 Mo12 S6 105.66(10) . 7_575 ? O13 Mo12 S6 84.97(10) 7_575 7_575 ? O13 Mo12 S6 144.94(10) . 7_575 ? S6 Mo12 S6 102.61(6) . 7_575 ? O12 Mo12 Mo11 104.07(16) . . ? O13 Mo12 Mo11 133.30(9) 7_575 . ? O13 Mo12 Mo11 133.30(9) . . ? S6 Mo12 Mo11 52.22(3) . . ? S6 Mo12 Mo11 52.22(3) 7_575 . ? Mo1 S1 Mo2 73.89(4) . . ? Mo4 S2 Mo3 74.78(4) . . ? Mo5 S3 Mo6 74.81(4) . . ? Mo7 S4 Mo8 74.08(4) . . ? Mo9 S5 Mo10 74.71(4) . . ? Mo12 S6 Mo11 75.76(4) . . ? Mo12 O13 Mo1 107.73(15) . . ? Mo3 O14 Mo2 101.26(15) . . ? Mo4 O15 Mo5 105.19(14) . . ? Mo6 O16 Mo7 107.94(14) . . ? Mo9 O17 Mo8 105.59(14) . . ? Mo11 O18 Mo10 103.21(16) . . ? C1 O19 Mo1 126.0(4) . . ? C1 O20 Mo2 125.4(4) . . ? C1 O20 Mo3 148.9(4) . . ? Mo2 O20 Mo3 85.72(14) . . ? C6 O21 Mo7 124.0(4) . . ? C6 O22 Mo8 125.2(4) . . ? O19 C1 O20 122.5(6) . . ? O19 C1 C2 119.6(5) . . ? O20 C1 C2 117.9(5) . . ? C1 C2 C3 115.1(5) . . ? C1 C2 H2A 108.5 . . ? C3 C2 H2A 108.5 . . ? C1 C2 H2B 108.5 . . ? C3 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? C2 C3 C4 116.3(6) . . ? C2 C3 H3A 108.2 . . ? C4 C3 H3A 108.2 . . ? C2 C3 H3B 108.2 . . ? C4 C3 H3B 108.2 . . ? H3A C3 H3B 107.4 . . ? C5 C4 C3 110.6(6) . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 119.7(6) . . ? C4 C5 H5A 107.4 . . ? C6 C5 H5A 107.4 . . ? C4 C5 H5B 107.4 . . ? C6 C5 H5B 107.4 . . ? H5A C5 H5B 106.9 . . ? O21 C6 O22 124.9(6) . . ? O21 C6 C5 119.8(6) . . ? O22 C6 C5 115.3(5) . . ? C11 N7 C9 108.9(4) . . ? C11 N7 C10 111.0(4) . . ? C9 N7 C10 109.7(4) . . ? C11 N7 C8 108.8(4) . . ? C9 N7 C8 110.4(4) . . ? C10 N7 C8 108.1(4) . . ? N7 C8 H8A 109.5 . . ? N7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N7 C9 H9A 109.5 . . ? N7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N7 C10 H10A 109.5 . . ? N7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N7 C11 H11A 109.5 . . ? N7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O19W O19W O18W 131.0(6) 7_575 . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.041 _refine_diff_density_min -1.408 _refine_diff_density_rms 0.379 #===END data_Mo12Sub _database_code_depnum_ccdc_archive 'CCDC 640034' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 K2 Mo12 O56 S12' _chemical_formula_weight 2606.28 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' 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' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(2)/mnm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y, x, -z' '-y, -x, -z' '-x, -y, -z' 'x, y, -z' 'y-1/2, -x-1/2, -z-1/2' '-y-1/2, x-1/2, -z-1/2' 'x-1/2, -y-1/2, z-1/2' '-x-1/2, y-1/2, z-1/2' '-y, -x, z' 'y, x, z' _cell_length_a 18.4395(4) _cell_length_b 18.4395(4) _cell_length_c 11.5430(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3924.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9658 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 30.04 _exptl_crystal_description parallelepiped _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.205 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2460 _exptl_absorpt_coefficient_mu 2.364 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6007 _exptl_absorpt_correction_T_max 0.7645 _exptl_absorpt_process_details 'SADABS (Sheldrick, V2.10)' _exptl_special_details ; 'Blessing, Acta Cryst. (1995) A51, 33-38' ; _diffrn_ambient_temperature 293(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 'phi and omega scans' _diffrn_detector_area_resol_mean 512x512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 71533 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0140 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 30.04 _reflns_number_total 3122 _reflns_number_gt 2689 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0607P)^2^+9.4959P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens none _refine_ls_hydrogen_treatment none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3122 _refine_ls_number_parameters 122 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0437 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.1221 _refine_ls_wR_factor_gt 0.0988 _refine_ls_goodness_of_fit_ref 1.213 _refine_ls_restrained_S_all 1.445 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.735771(11) 0.388354(11) 0.0000 0.02599(5) Uani 1 2 d S . . Mo2 Mo 0.816559(11) 0.517871(12) 0.0000 0.02849(5) Uani 1 2 d S . . Mo3 Mo 0.804600(13) 0.697252(12) 0.0000 0.03340(5) Uani 1 2 d S . . S1 S 0.75879(3) 0.46236(3) 0.15525(4) 0.03788(11) Uani 1 1 d . . . S2 S 0.74802(3) 0.74802(3) -0.16045(6) 0.03687(15) Uani 1 2 d S . . O1 O 0.80130(11) 0.32480(11) 0.0000 0.0390(5) Uani 1 2 d S . . O2 O 0.89987(11) 0.48163(12) 0.0000 0.0406(5) Uani 1 2 d S . . O3 O 0.88435(12) 0.74202(14) 0.0000 0.0509(7) Uani 1 2 d S . . O4 O 0.65289(8) 0.34711(8) 0.10027(15) 0.0351(4) Uani 1 2 d S . . O5 O 0.83244(9) 0.60818(7) -0.10506(13) 0.0423(4) Uani 1 1 d . . . O6 O 0.70543(16) 0.61913(13) 0.0000 0.0630(7) Uani 1 2 d S . . C1 C 0.64058(16) 0.64058(16) 0.0000 0.0958(19) Uani 1 4 d SD . . C2 C 0.6302(3) 0.5585(4) -0.0153(15) 0.34(2) Uiso 0.25 1 d PD . . C3 C 0.5228(3) 0.5671(3) -0.0481(5) 0.108(4) Uiso 0.38 1 d PD . . C4 C 0.5000 0.5000 -0.1240(11) 0.151(9) Uiso 0.50 4 d SPD . . K1 K 0.61857(9) 0.38143(9) 0.3205(2) 0.0632(6) Uani 0.10 2 d SP . . K2 K 0.99042(8) 0.61626(10) -0.11483(16) 0.0666(5) Uani 0.10 1 d P . . K3 K 0.78286(12) 0.59502(9) -0.32676(15) 0.0730(6) Uani 0.10 1 d P . . O1W O 0.61857(9) 0.38143(9) 0.3205(2) 0.0632(6) Uani 0.90 2 d SP . . O2W O 0.99042(8) 0.61626(10) -0.11483(16) 0.0666(5) Uani 0.90 1 d P . . O3W O 0.78286(12) 0.59502(9) -0.32676(15) 0.0730(6) Uani 0.90 1 d P . . O4W O 0.53241(11) 0.64327(12) -0.37945(18) 0.0676(6) Uani 1 1 d . . . O5W O 1.0000 0.5000 -0.2500 0.0964(19) Uani 1 4 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 Mo1 0.02669(8) 0.02905(9) 0.02223(8) 0.000 0.000 0.00016(7) Mo2 0.02606(8) 0.03006(9) 0.02936(9) 0.000 0.000 -0.00091(7) Mo3 0.03548(10) 0.02621(9) 0.03850(10) 0.000 0.000 0.00100(8) S1 0.0477(2) 0.0407(2) 0.02526(17) -0.00394(17) 0.00162(17) -0.01147(19) S2 0.03671(18) 0.03671(18) 0.0372(3) 0.00342(18) 0.00342(18) 0.0011(3) O1 0.0372(9) 0.0370(9) 0.0428(10) 0.000 0.000 0.0089(8) O2 0.0287(8) 0.0423(10) 0.0509(11) 0.000 0.000 0.0024(8) O3 0.0349(10) 0.0525(12) 0.0654(14) 0.000 0.000 0.0010(9) O4 0.0397(5) 0.0397(5) 0.0261(7) -0.0051(5) 0.0051(5) -0.0080(7) O5 0.0592(8) 0.0334(6) 0.0343(6) 0.0016(5) 0.0015(6) 0.0073(6) O6 0.0865(15) 0.0496(11) 0.0531(13) 0.000 0.000 -0.0392(10) C1 0.0926(16) 0.0926(16) 0.102(5) 0.000 0.000 -0.077(2) K1 0.0714(8) 0.0714(8) 0.0468(10) -0.0020(7) 0.0020(7) 0.0106(11) K2 0.0421(7) 0.0825(10) 0.0753(10) 0.0226(8) 0.0052(7) 0.0007(7) K3 0.1041(13) 0.0598(9) 0.0553(8) 0.0102(7) 0.0022(9) -0.0007(9) O1W 0.0714(8) 0.0714(8) 0.0468(10) -0.0020(7) 0.0020(7) 0.0106(11) O2W 0.0421(7) 0.0825(10) 0.0753(10) 0.0226(8) 0.0052(7) 0.0007(7) O3W 0.1041(13) 0.0598(9) 0.0553(8) 0.0102(7) 0.0022(9) -0.0007(9) O4W 0.0665(11) 0.0766(12) 0.0598(10) -0.0059(10) 0.0092(9) 0.0055(10) O5W 0.102(2) 0.102(2) 0.086(3) 0.000 0.000 0.000 _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 1.683(2) . ? Mo1 O4 2.0624(11) . ? Mo1 O4 2.0624(11) 10 ? Mo1 S1 2.2922(5) . ? Mo1 S1 2.2922(5) 10 ? Mo1 Mo2 2.8148(3) . ? Mo2 O2 1.675(2) . ? Mo2 O5 2.0807(14) 10 ? Mo2 O5 2.0807(14) . ? Mo2 S1 2.3225(5) 10 ? Mo2 S1 2.3225(5) . ? Mo2 K2 3.9148(16) 10 ? Mo2 K2 3.9149(16) . ? Mo2 K3 4.0787(18) . ? Mo2 K3 4.0787(18) 10 ? Mo3 O3 1.686(2) . ? Mo3 O5 2.1052(14) 10 ? Mo3 O5 2.1052(14) . ? Mo3 S2 2.3227(6) 10 ? Mo3 S2 2.3227(6) . ? Mo3 O6 2.328(3) . ? Mo3 Mo3 2.7993(5) 7 ? Mo3 K2 3.9658(16) 10 ? Mo3 K2 3.9658(16) . ? S1 K3 3.1780(18) 10 ? S1 K1 3.5427(15) . ? S1 K2 3.5525(19) 3_645 ? S2 Mo3 2.3227(6) 7 ? S2 K3 3.4724(18) . ? S2 K3 3.4724(18) 16 ? S2 K1 3.486(2) 4_564 ? O1 K3 2.873(2) 3_645 ? O1 K3 2.873(2) 12_755 ? O2 K2 3.018(3) 9_765 ? O2 K2 3.018(3) 2_765 ? O2 K2 3.272(3) 10 ? O2 K2 3.272(3) . ? O3 K1 3.302(3) 11_676 ? O3 K1 3.302(3) 4_564 ? O3 K2 3.311(3) 10 ? O3 K2 3.311(3) . ? O4 Mo1 2.0624(11) 15_665 ? O4 K1 2.695(3) . ? O5 K3 2.728(2) . ? O5 K2 2.919(2) . ? O6 C1 1.260(4) . ? O6 C2 1.790(7) 10 ? O6 C2 1.790(7) . ? C1 O6 1.260(3) 7 ? C1 C2 1.535(8) 10 ? C1 C2 1.535(8) 7 ? C1 C2 1.535(8) 16 ? C1 C2 1.535(8) . ? C2 C2 0.35(3) 10 ? C2 C3 1.390(9) 16 ? C2 C3 1.525(11) 7 ? C2 C2 1.868(13) 16 ? C2 C2 1.901(15) 7 ? C2 C3 2.022(8) . ? C3 C3 1.110(11) 10 ? C3 C3 1.155(10) 16 ? C3 C2 1.390(9) 16 ? C3 C2 1.525(11) 7 ? C3 C4 1.573(8) . ? C3 C3 1.602(10) 7 ? C4 C3 1.573(8) 2_665 ? C4 C3 1.573(8) 16 ? C4 C3 1.573(8) 15_665 ? K1 O4W 2.902(3) 9_665 ? K1 O4W 2.902(3) 7 ? K1 O3 3.302(3) 5_645 ? K1 O3 3.302(3) 3_645 ? K1 S2 3.486(2) 3_645 ? K1 S1 3.5427(14) 15_665 ? K1 K1 4.144(5) 10_556 ? K1 K3 4.9693(19) 8_665 ? K1 K3 4.9693(19) 10 ? K2 O2W 2.651(4) 10 ? K2 K2 2.651(4) 10 ? K2 O5W 2.6573(19) . ? K2 O3W 2.763(3) 11_675 ? K2 K3 2.763(3) 11_675 ? K2 O2 3.018(3) 9_765 ? K2 S1 3.5524(19) 4_564 ? K3 O2W 2.763(3) 12_755 ? K3 K2 2.763(3) 12_755 ? K3 O1 2.873(2) 11_675 ? K3 O4W 2.886(3) 16 ? K3 S1 3.1780(18) 10 ? K3 K3 3.999(4) 10_554 ? K3 K2 4.271(3) 3_644 ? K3 K3 4.898(4) 16 ? O4W K3 2.886(3) 16 ? O4W K1 2.902(3) 9_665 ? O5W K2 2.6573(19) 2_765 ? O5W K2 2.6573(19) 12_755 ? O5W K2 2.6573(19) 11_675 ? 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 O4 105.97(8) . . ? O1 Mo1 O4 105.97(8) . 10 ? O4 Mo1 O4 68.28(8) . 10 ? O1 Mo1 S1 106.35(4) . . ? O4 Mo1 S1 85.30(4) . . ? O4 Mo1 S1 142.71(6) 10 . ? O1 Mo1 S1 106.35(4) . 10 ? O4 Mo1 S1 142.71(6) . 10 ? O4 Mo1 S1 85.30(4) 10 10 ? S1 Mo1 S1 102.85(3) . 10 ? O1 Mo1 Mo2 102.17(7) . . ? O4 Mo1 Mo2 134.83(4) . . ? O4 Mo1 Mo2 134.83(4) 10 . ? S1 Mo1 Mo2 52.904(13) . . ? S1 Mo1 Mo2 52.903(13) 10 . ? O2 Mo2 O5 100.97(8) . 10 ? O2 Mo2 O5 100.97(8) . . ? O5 Mo2 O5 71.30(8) 10 . ? O2 Mo2 S1 104.17(5) . 10 ? O5 Mo2 S1 150.11(5) 10 10 ? O5 Mo2 S1 88.14(4) . 10 ? O2 Mo2 S1 104.17(5) . . ? O5 Mo2 S1 88.14(4) 10 . ? O5 Mo2 S1 150.11(5) . . ? S1 Mo2 S1 101.00(3) 10 . ? O2 Mo2 Mo1 98.45(7) . . ? O5 Mo2 Mo1 138.89(4) 10 . ? O5 Mo2 Mo1 138.89(4) . . ? S1 Mo2 Mo1 51.927(13) 10 . ? S1 Mo2 Mo1 51.926(13) . . ? O2 Mo2 K2 55.52(7) . 10 ? O5 Mo2 K2 46.89(5) 10 10 ? O5 Mo2 K2 73.22(5) . 10 ? S1 Mo2 K2 147.26(3) 10 10 ? S1 Mo2 K2 108.58(3) . 10 ? Mo1 Mo2 K2 145.75(3) . 10 ? O2 Mo2 K2 55.52(7) . . ? O5 Mo2 K2 73.22(5) 10 . ? O5 Mo2 K2 46.89(5) . . ? S1 Mo2 K2 108.58(3) 10 . ? S1 Mo2 K2 147.26(3) . . ? Mo1 Mo2 K2 145.75(3) . . ? K2 Mo2 K2 39.58(5) 10 . ? O2 Mo2 K3 106.19(4) . . ? O5 Mo2 K3 106.34(5) 10 . ? O5 Mo2 K3 37.19(5) . . ? S1 Mo2 K3 50.97(3) 10 . ? S1 Mo2 K3 142.88(3) . . ? Mo1 Mo2 K3 102.43(3) . . ? K2 Mo2 K3 106.04(4) 10 . ? K2 Mo2 K3 69.51(4) . . ? O2 Mo2 K3 106.19(4) . 10 ? O5 Mo2 K3 37.19(5) 10 10 ? O5 Mo2 K3 106.34(5) . 10 ? S1 Mo2 K3 142.88(3) 10 10 ? S1 Mo2 K3 50.97(3) . 10 ? Mo1 Mo2 K3 102.43(3) . 10 ? K2 Mo2 K3 69.51(4) 10 10 ? K2 Mo2 K3 106.04(4) . 10 ? K3 Mo2 K3 135.26(5) . 10 ? O3 Mo3 O5 99.75(8) . 10 ? O3 Mo3 O5 99.75(8) . . ? O5 Mo3 O5 70.35(8) 10 . ? O3 Mo3 S2 101.21(5) . 10 ? O5 Mo3 S2 87.97(4) 10 10 ? O5 Mo3 S2 152.04(4) . 10 ? O3 Mo3 S2 101.21(5) . . ? O5 Mo3 S2 152.04(4) 10 . ? O5 Mo3 S2 87.97(4) . . ? S2 Mo3 S2 105.76(2) 10 . ? O3 Mo3 O6 171.08(11) . . ? O5 Mo3 O6 73.07(7) 10 . ? O5 Mo3 O6 73.07(7) . . ? S2 Mo3 O6 84.06(4) 10 . ? S2 Mo3 O6 84.06(4) . . ? O3 Mo3 Mo3 105.69(9) . 7 ? O5 Mo3 Mo3 136.39(4) 10 7 ? O5 Mo3 Mo3 136.39(4) . 7 ? S2 Mo3 Mo3 52.943(12) 10 7 ? S2 Mo3 Mo3 52.943(12) . 7 ? O6 Mo3 Mo3 83.23(7) . 7 ? O3 Mo3 K2 55.32(8) . 10 ? O5 Mo3 K2 45.81(5) 10 10 ? O5 Mo3 K2 71.82(5) . 10 ? S2 Mo3 K2 105.87(3) 10 10 ? S2 Mo3 K2 143.74(3) . 10 ? O6 Mo3 K2 116.47(7) . 10 ? Mo3 Mo3 K2 151.31(3) 7 10 ? O3 Mo3 K2 55.32(8) . . ? O5 Mo3 K2 71.82(5) 10 . ? O5 Mo3 K2 45.81(5) . . ? S2 Mo3 K2 143.74(3) 10 . ? S2 Mo3 K2 105.86(3) . . ? O6 Mo3 K2 116.47(7) . . ? Mo3 Mo3 K2 151.31(3) 7 . ? K2 Mo3 K2 39.05(5) 10 . ? Mo1 S1 Mo2 75.170(15) . . ? Mo1 S1 K3 166.20(4) . 10 ? Mo2 S1 K3 94.44(4) . 10 ? Mo1 S1 K1 92.01(3) . . ? Mo2 S1 K1 159.37(4) . . ? K3 S1 K1 95.21(5) 10 . ? Mo1 S1 K2 142.27(3) . 3_645 ? Mo2 S1 K2 102.40(3) . 3_645 ? K3 S1 K2 48.08(5) 10 3_645 ? K1 S1 K2 97.61(5) . 3_645 ? Mo3 S2 Mo3 74.11(2) 7 . ? Mo3 S2 K3 151.68(4) 7 . ? Mo3 S2 K3 91.73(3) . . ? Mo3 S2 K3 91.73(3) 7 16 ? Mo3 S2 K3 151.68(4) . 16 ? K3 S2 K3 89.71(7) . 16 ? Mo3 S2 K1 91.02(4) 7 4_564 ? Mo3 S2 K1 91.02(4) . 4_564 ? K3 S2 K1 114.07(5) . 4_564 ? K3 S2 K1 114.07(4) 16 4_564 ? Mo1 O1 K3 131.70(6) . 3_645 ? Mo1 O1 K3 131.70(6) . 12_755 ? K3 O1 K3 88.23(9) 3_645 12_755 ? Mo2 O2 K2 148.57(7) . 9_765 ? Mo2 O2 K2 148.57(7) . 2_765 ? K2 O2 K2 52.11(8) 9_765 2_765 ? Mo2 O2 K2 99.51(9) . 10 ? K2 O2 K2 86.20(7) 9_765 10 ? K2 O2 K2 106.83(7) 2_765 10 ? Mo2 O2 K2 99.51(9) . . ? K2 O2 K2 106.83(7) 9_765 . ? K2 O2 K2 86.20(7) 2_765 . ? K2 O2 K2 47.79(7) 10 . ? Mo3 O3 K1 111.52(9) . 11_676 ? Mo3 O3 K1 111.52(9) . 4_564 ? K1 O3 K1 77.73(9) 11_676 4_564 ? Mo3 O3 K2 99.92(10) . 10 ? K1 O3 K2 107.68(5) 11_676 10 ? K1 O3 K2 143.72(8) 4_564 10 ? Mo3 O3 K2 99.92(10) . . ? K1 O3 K2 143.72(8) 11_676 . ? K1 O3 K2 107.68(5) 4_564 . ? K2 O3 K2 47.20(7) 10 . ? Mo1 O4 Mo1 103.39(8) 15_665 . ? Mo1 O4 K1 128.08(4) 15_665 . ? Mo1 O4 K1 128.08(4) . . ? Mo2 O5 Mo3 104.73(7) . . ? Mo2 O5 K3 115.36(7) . . ? Mo3 O5 K3 121.87(7) . . ? Mo2 O5 K2 101.76(7) . . ? Mo3 O5 K2 103.05(7) . . ? K3 O5 K2 107.62(8) . . ? C1 O6 C2 57.3(3) . 10 ? C1 O6 C2 57.3(3) . . ? C2 O6 C2 11.3(11) 10 . ? C1 O6 Mo3 123.5(2) . . ? C2 O6 Mo3 174.3(6) 10 . ? C2 O6 Mo3 174.3(5) . . ? O6 C1 O6 126.6(4) 7 . ? O6 C1 C2 153.7(4) 7 10 ? O6 C1 C2 79.0(3) . 10 ? O6 C1 C2 79.0(3) 7 7 ? O6 C1 C2 153.7(4) . 7 ? C2 C1 C2 75.0(5) 10 7 ? O6 C1 C2 79.0(3) 7 16 ? O6 C1 C2 153.7(4) . 16 ? C2 C1 C2 76.5(5) 10 16 ? C2 C1 C2 13.2(13) 7 16 ? O6 C1 C2 153.7(4) 7 . ? O6 C1 C2 79.0(3) . . ? C2 C1 C2 13.2(13) 10 . ? C2 C1 C2 76.5(5) 7 . ? C2 C1 C2 75.0(5) 16 . ? C2 C2 C3 105.8(7) 10 16 ? C2 C2 C3 61.3(6) 10 7 ? C3 C2 C3 44.5(5) 16 7 ? C2 C2 C1 83.4(6) 10 . ? C3 C2 C1 127.1(6) 16 . ? C3 C2 C1 117.8(8) 7 . ? C2 C2 O6 84.3(5) 10 . ? C3 C2 O6 166.4(10) 16 . ? C3 C2 O6 144.5(11) 7 . ? C1 C2 O6 43.7(2) . . ? C2 C2 C2 90.001(3) 10 16 ? C3 C2 C2 75.1(4) 16 16 ? C3 C2 C2 76.5(3) 7 16 ? C1 C2 C2 52.5(3) . 16 ? O6 C2 C2 96.1(2) . 16 ? C2 C2 C2 79.3(10) 10 7 ? C3 C2 C2 78.4(4) 16 7 ? C3 C2 C2 71.4(6) 7 7 ? C1 C2 C2 51.7(3) . 7 ? O6 C2 C2 95.0(3) . 7 ? C2 C2 C2 10.7(10) 16 7 ? C2 C2 C3 100.8(5) 10 . ? C3 C2 C3 33.5(4) 16 . ? C3 C2 C3 51.4(4) 7 . ? C1 C2 C3 93.9(4) . . ? O6 C2 C3 136.8(4) . . ? C2 C2 C3 41.6(3) 16 . ? C2 C2 C3 45.6(3) 7 . ? C3 C3 C3 89.996(1) 10 16 ? C3 C3 C2 74.2(7) 10 16 ? C3 C3 C2 104.9(4) 16 16 ? C3 C3 C2 61.3(6) 10 7 ? C3 C3 C2 103.5(3) 16 7 ? C2 C3 C2 12.9(13) 16 7 ? C3 C3 C4 123.8(4) 10 . ? C3 C3 C4 68.5(2) 16 . ? C2 C3 C4 159.5(8) 16 . ? C2 C3 C4 169.5(6) 7 . ? C3 C3 C3 46.1(4) 10 7 ? C3 C3 C3 43.9(4) 16 7 ? C2 C3 C3 89.8(6) 16 7 ? C2 C3 C3 80.6(5) 7 7 ? C4 C3 C3 97.0(4) . 7 ? C3 C3 C2 79.2(5) 10 . ? C3 C3 C2 41.6(3) 16 . ? C2 C3 C2 63.2(5) 16 . ? C2 C3 C2 63.0(5) 7 . ? C4 C3 C2 107.7(4) . . ? C3 C3 C2 48.1(4) 7 . ? C3 C4 C3 112.3(8) 2_665 . ? C3 C4 C3 96.3(7) 2_665 16 ? C3 C4 C3 43.1(4) . 16 ? C3 C4 C3 43.1(4) 2_665 15_665 ? C3 C4 C3 96.3(7) . 15_665 ? C3 C4 C3 112.3(8) 16 15_665 ? O4 K1 O4W 114.18(7) . 9_665 ? O4 K1 O4W 114.18(7) . 7 ? O4W K1 O4W 104.26(11) 9_665 7 ? O4 K1 O3 114.38(8) . 5_645 ? O4W K1 O3 73.44(6) 9_665 5_645 ? O4W K1 O3 127.03(9) 7 5_645 ? O4 K1 O3 114.38(8) . 3_645 ? O4W K1 O3 127.03(9) 9_665 3_645 ? O4W K1 O3 73.44(6) 7 3_645 ? O3 K1 O3 68.38(8) 5_645 3_645 ? O4 K1 S2 74.22(7) . 3_645 ? O4W K1 S2 123.46(6) 9_665 3_645 ? O4W K1 S2 123.46(6) 7 3_645 ? O3 K1 S2 54.73(5) 5_645 3_645 ? O3 K1 S2 54.73(5) 3_645 3_645 ? O4 K1 S1 54.53(3) . . ? O4W K1 S1 153.20(9) 9_665 . ? O4W K1 S1 66.89(5) 7 . ? O3 K1 S1 132.66(8) 5_645 . ? O3 K1 S1 76.28(4) 3_645 . ? S2 K1 S1 79.41(4) 3_645 . ? O4 K1 S1 54.53(3) . 15_665 ? O4W K1 S1 66.89(5) 9_665 15_665 ? O4W K1 S1 153.20(9) 7 15_665 ? O3 K1 S1 76.28(4) 5_645 15_665 ? O3 K1 S1 132.66(8) 3_645 15_665 ? S2 K1 S1 79.41(4) 3_645 15_665 ? S1 K1 S1 108.96(6) . 15_665 ? O4 K1 K1 160.60(7) . 10_556 ? O4W K1 K1 76.44(6) 9_665 10_556 ? O4W K1 K1 76.44(6) 7 10_556 ? O3 K1 K1 51.13(5) 5_645 10_556 ? O3 K1 K1 51.13(5) 3_645 10_556 ? S2 K1 K1 86.38(4) 3_645 10_556 ? S1 K1 K1 122.57(3) . 10_556 ? S1 K1 K1 122.58(3) 15_665 10_556 ? O4 K1 K3 93.25(4) . 8_665 ? O4W K1 K3 30.75(5) 9_665 8_665 ? O4W K1 K3 134.90(8) 7 8_665 ? O3 K1 K3 60.22(4) 5_645 8_665 ? O3 K1 K3 128.15(6) 3_645 8_665 ? S2 K1 K3 97.36(4) 3_645 8_665 ? S1 K1 K3 147.47(6) . 8_665 ? S1 K1 K3 39.56(2) 15_665 8_665 ? K1 K1 K3 89.17(3) 10_556 8_665 ? O4 K1 K3 93.25(4) . 10 ? O4W K1 K3 134.90(8) 9_665 10 ? O4W K1 K3 30.74(5) 7 10 ? O3 K1 K3 128.15(6) 5_645 10 ? O3 K1 K3 60.22(4) 3_645 10 ? S2 K1 K3 97.36(4) 3_645 10 ? S1 K1 K3 39.56(2) . 10 ? S1 K1 K3 147.47(6) 15_665 10 ? K1 K1 K3 89.17(3) 10_556 10 ? K3 K1 K3 165.04(7) 8_665 10 ? O2W K2 K2 0.00(8) 10 10 ? O2W K2 O5W 125.96(4) 10 . ? K2 K2 O5W 125.96(4) 10 . ? O2W K2 O3W 104.12(5) 10 11_675 ? K2 K2 O3W 104.12(5) 10 11_675 ? O5W K2 O3W 110.70(7) . 11_675 ? O2W K2 K3 104.12(5) 10 11_675 ? K2 K2 K3 104.12(5) 10 11_675 ? O5W K2 K3 110.70(7) . 11_675 ? O3W K2 K3 0.00(10) 11_675 11_675 ? O2W K2 O5 87.79(5) 10 . ? K2 K2 O5 87.79(5) 10 . ? O5W K2 O5 92.74(6) . . ? O3W K2 O5 137.76(8) 11_675 . ? K3 K2 O5 137.76(8) 11_675 . ? O2W K2 O2 63.95(4) 10 9_765 ? K2 K2 O2 63.95(4) 10 9_765 ? O5W K2 O2 74.38(5) . 9_765 ? O3W K2 O2 92.40(7) 11_675 9_765 ? K3 K2 O2 92.40(7) 11_675 9_765 ? O5 K2 O2 128.43(8) . 9_765 ? O2W K2 O2 66.10(4) 10 . ? K2 K2 O2 66.10(4) 10 . ? O5W K2 O2 70.11(5) . . ? O3W K2 O2 164.96(8) 11_675 . ? K3 K2 O2 164.96(8) 11_675 . ? O5 K2 O2 55.70(5) . . ? O2 K2 O2 73.17(7) 9_765 . ? O2W K2 O3 66.40(4) 10 . ? K2 K2 O3 66.40(4) 10 . ? O5W K2 O3 147.08(7) . . ? O3W K2 O3 92.21(8) 11_675 . ? K3 K2 O3 92.21(8) 11_675 . ? O5 K2 O3 55.30(6) . . ? O2 K2 O3 129.73(7) 9_765 . ? O2 K2 O3 93.89(7) . . ? O2W K2 S1 138.34(3) 10 4_564 ? K2 K2 S1 138.34(3) 10 4_564 ? O5W K2 S1 95.41(5) . 4_564 ? O3W K2 S1 58.85(5) 11_675 4_564 ? K3 K2 S1 58.85(5) 11_675 4_564 ? O5 K2 S1 85.22(5) . 4_564 ? O2 K2 S1 144.45(6) 9_765 4_564 ? O2 K2 S1 136.08(6) . 4_564 ? O3 K2 S1 76.04(4) . 4_564 ? O2W K2 Mo2 70.21(3) 10 . ? K2 K2 Mo2 70.21(3) 10 . ? O5W K2 Mo2 83.07(4) . . ? O3W K2 Mo2 165.06(8) 11_675 . ? K3 K2 Mo2 165.06(8) 11_675 . ? O5 K2 Mo2 31.36(3) . . ? O2 K2 Mo2 97.07(6) 9_765 . ? O2 K2 Mo2 24.96(4) . . ? O3 K2 Mo2 72.86(5) . . ? S1 K2 Mo2 115.74(4) 4_564 . ? O2W K2 Mo3 70.47(3) 10 . ? K2 K2 Mo3 70.47(3) 10 . ? O5W K2 Mo3 123.88(5) . . ? O3W K2 Mo3 115.54(7) 11_675 . ? K3 K2 Mo3 115.54(7) 11_675 . ? O5 K2 Mo3 31.14(3) . . ? O2 K2 Mo3 131.12(6) 9_765 . ? O2 K2 Mo3 73.11(5) . . ? O3 K2 Mo3 24.76(4) . . ? S1 K2 Mo3 83.09(4) 4_564 . ? Mo2 K2 Mo3 49.75(2) . . ? O5 K3 O2W 93.75(8) . 12_755 ? O5 K3 K2 93.75(8) . 12_755 ? O2W K3 K2 0.00(10) 12_755 12_755 ? O5 K3 O1 120.24(8) . 11_675 ? O2W K3 O1 96.51(8) 12_755 11_675 ? K2 K3 O1 96.51(8) 12_755 11_675 ? O5 K3 O4W 122.15(9) . 16 ? O2W K3 O4W 105.65(8) 12_755 16 ? K2 K3 O4W 105.65(8) 12_755 16 ? O1 K3 O4W 111.08(8) 11_675 16 ? O5 K3 S1 62.03(5) . 10 ? O2W K3 S1 73.07(6) 12_755 10 ? K2 K3 S1 73.07(6) 12_755 10 ? O1 K3 S1 169.58(9) 11_675 10 ? O4W K3 S1 72.47(6) 16 10 ? O5 K3 S2 58.07(5) . . ? O2W K3 S2 145.75(8) 12_755 . ? K2 K3 S2 145.75(8) 12_755 . ? O1 K3 S2 83.91(5) 11_675 . ? O4W K3 S2 106.05(8) 16 . ? S1 K3 S2 104.78(5) 10 . ? O5 K3 K3 159.72(6) . 10_554 ? O2W K3 K3 75.88(5) 12_755 10_554 ? K2 K3 K3 75.88(5) 12_755 10_554 ? O1 K3 K3 45.88(5) 11_675 10_554 ? O4W K3 K3 77.83(5) 16 10_554 ? S1 K3 K3 128.53(3) 10 10_554 ? S2 K3 K3 123.56(3) . 10_554 ? O5 K3 Mo2 27.45(3) . . ? O2W K3 Mo2 83.09(6) 12_755 . ? K2 K3 Mo2 83.09(6) 12_755 . ? O1 K3 Mo2 146.60(7) 11_675 . ? O4W K3 Mo2 101.03(6) 16 . ? S1 K3 Mo2 34.59(2) 10 . ? S2 K3 Mo2 78.48(4) . . ? K3 K3 Mo2 157.63(3) 10_554 . ? O5 K3 K2 128.65(8) . 3_644 ? O2W K3 K2 37.01(6) 12_755 3_644 ? K2 K3 K2 37.01(6) 12_755 3_644 ? O1 K3 K2 68.98(5) 11_675 3_644 ? O4W K3 K2 92.51(7) 16 3_644 ? S1 K3 K2 101.43(5) 10 3_644 ? S2 K3 K2 151.40(6) . 3_644 ? K3 K3 K2 38.86(3) 10_554 3_644 ? Mo2 K3 K2 119.75(5) . 3_644 ? O5 K3 K2 37.61(5) . . ? O2W K3 K2 68.02(7) 12_755 . ? K2 K3 K2 68.02(7) 12_755 . ? O1 K3 K2 95.18(7) 11_675 . ? O4W K3 K2 153.66(7) 16 . ? S1 K3 K2 81.32(5) 10 . ? S2 K3 K2 77.81(4) . . ? K3 K3 K2 122.45(3) 10_554 . ? Mo2 K3 K2 53.55(3) . . ? K2 K3 K2 95.22(5) 3_644 . ? O5 K3 K3 100.02(5) . 16 ? O2W K3 K3 165.84(5) 12_755 16 ? K2 K3 K3 165.84(5) 12_755 16 ? O1 K3 K3 73.72(6) 11_675 16 ? O4W K3 K3 69.65(6) 16 16 ? S1 K3 K3 116.46(4) 10 16 ? S2 K3 K3 45.14(4) . 16 ? K3 K3 K3 90.0 10_554 16 ? Mo2 K3 K3 110.75(3) . 16 ? K2 K3 K3 128.86(3) 3_644 16 ? K2 K3 K3 122.20(3) . 16 ? K3 O4W K1 118.32(9) 16 9_665 ? K2 O5W K2 110.17(4) 2_765 12_755 ? K2 O5W K2 110.17(4) 2_765 11_675 ? K2 O5W K2 108.09(8) 12_755 11_675 ? K2 O5W K2 108.09(8) 2_765 . ? K2 O5W K2 110.17(4) 12_755 . ? K2 O5W K2 110.17(4) 11_675 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.04 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.843 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.175 #===END data_Mo14Azel _database_code_depnum_ccdc_archive 'CCDC 640035' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H38 Mo14 N2 O60 S14' _chemical_formula_weight 3022.49 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 13.0709(3) _cell_length_b 27.1242(5) _cell_length_c 30.5257(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.8990(10) _cell_angle_gamma 90.00 _cell_volume 10719.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 9433 _cell_measurement_theta_min 2.33 _cell_measurement_theta_max 29.99 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.873 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5784 _exptl_absorpt_coefficient_mu 1.928 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5127 _exptl_absorpt_correction_T_max 0.6548 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 125505 _diffrn_reflns_av_R_equivalents 0.0297 _diffrn_reflns_av_sigmaI/netI 0.0165 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 30.08 _reflns_number_total 15730 _reflns_number_gt 12597 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0660P)^2^+84.7282P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15730 _refine_ls_number_parameters 523 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0685 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1632 _refine_ls_wR_factor_gt 0.1359 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.171 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 0.43683(3) 0.262905(13) 0.198298(11) 0.04244(8) Uani 1 1 d . . . Mo2 Mo 0.35521(3) 0.321836(13) 0.125341(11) 0.04308(8) Uani 1 1 d . . . Mo3 Mo 0.28611(2) 0.408313(13) 0.048111(11) 0.04195(7) Uani 1 1 d . . . Mo4 Mo 0.25264(3) 0.499294(12) 0.003465(11) 0.04024(7) Uani 1 1 d . . . Mo5 Mo 0.29191(2) 0.614554(12) 0.032549(11) 0.04080(7) Uani 1 1 d . . . Mo6 Mo 0.36309(3) 0.676456(13) 0.104382(11) 0.04347(8) Uani 1 1 d . . . Mo7 Mo 0.45879(3) 0.713324(14) 0.205050(12) 0.04911(9) Uani 1 1 d . . . S1 S 0.27796(8) 0.30253(4) 0.18746(4) 0.0488(2) Uani 1 1 d . . . S2 S 0.52496(8) 0.29786(4) 0.14555(4) 0.0514(3) Uani 1 1 d . . . S3 S 0.14140(8) 0.45929(4) 0.04496(4) 0.0482(2) Uani 1 1 d . . . S4 S 0.40231(8) 0.45226(4) 0.01185(4) 0.0473(2) Uani 1 1 d . . . S5 S 0.20570(8) 0.63703(4) 0.09063(4) 0.0488(2) Uani 1 1 d . . . S6 S 0.46181(8) 0.63347(4) 0.06039(4) 0.0476(2) Uani 1 1 d . . . S7 S 0.62744(9) 0.69894(5) 0.23498(4) 0.0591(3) Uani 1 1 d . . . O1 O 0.4097(3) 0.20605(12) 0.17840(12) 0.0635(9) Uani 1 1 d . . . O2 O 0.3100(3) 0.27654(12) 0.09049(10) 0.0551(8) Uani 1 1 d . . . O3 O 0.2439(2) 0.36677(12) 0.00892(11) 0.0563(8) Uani 1 1 d . . . O4 O 0.2003(3) 0.48513(13) -0.04860(10) 0.0572(8) Uani 1 1 d . . . O5 O 0.2606(2) 0.65860(11) -0.00516(10) 0.0517(8) Uani 1 1 d . . . O6 O 0.3442(3) 0.73270(11) 0.08179(11) 0.0585(9) Uani 1 1 d . . . O7 O 0.4500(3) 0.77352(14) 0.19474(12) 0.0734(11) Uani 1 1 d . . . O8 O 0.4158(2) 0.25111(12) 0.26465(10) 0.0525(8) Uani 1 1 d . . . O9 O 0.2418(2) 0.37398(11) 0.10334(10) 0.0517(7) Uani 1 1 d . . . O10 O 0.4092(2) 0.36957(11) 0.08121(10) 0.0514(7) Uani 1 1 d . . . O11 O 0.1726(2) 0.56534(10) 0.01046(9) 0.0448(7) Uani 1 1 d . . . O12 O 0.3469(2) 0.56056(10) -0.00859(9) 0.0426(6) Uani 1 1 d . . . O13 O 0.3320(2) 0.68081(13) 0.16853(10) 0.0569(8) Uani 1 1 d . . . O14 O 0.4972(2) 0.68203(14) 0.14838(10) 0.0588(9) Uani 1 1 d . . . O15 O 0.5000 0.3345(2) 0.2500 0.0638(13) Uani 1 2 d S . . O16 O 0.4067(3) 0.39598(12) 0.16937(12) 0.0642(10) Uani 1 1 d . . . O17 O 0.3480(2) 0.46449(11) 0.10714(10) 0.0534(8) Uani 1 1 d . . . O18 O 0.3203(2) 0.53419(10) 0.06992(9) 0.0438(6) Uani 1 1 d . . . C1 C 0.3507(3) 0.51077(18) 0.10527(13) 0.0514(11) Uani 1 1 d D . . C2 C 0.3891(7) 0.5409(2) 0.14541(19) 0.105(2) Uani 1 1 d D . . H2A H 0.4595 0.5508 0.1432 0.126 Uiso 1 1 calc R . . H2B H 0.3478 0.5707 0.1445 0.126 Uiso 1 1 calc R . . C3 C 0.3879(7) 0.5175(3) 0.1892(2) 0.112(2) Uani 1 1 d D . . H3A H 0.4369 0.4904 0.1933 0.134 Uiso 1 1 calc R . . H3B H 0.3196 0.5049 0.1920 0.134 Uiso 1 1 calc R . . C4 C 0.4191(5) 0.5592(4) 0.2234(2) 0.149(3) Uani 1 1 d D . . H4A H 0.3855 0.5562 0.2497 0.178 Uiso 0.50 1 calc R . . H4B H 0.4081 0.5919 0.2108 0.178 Uiso 0.50 1 calc R . . H4A' H 0.4705 0.5799 0.2124 0.176 Uiso 0.50 1 calc R . . H4B' H 0.3587 0.5795 0.2252 0.176 Uiso 0.50 1 calc R . . C5 C 0.5379(7) 0.5442(5) 0.2318(3) 0.0915(19) Uani 0.50 1 d PD . . H5A H 0.5449 0.5088 0.2286 0.110 Uiso 0.50 1 calc PR . . H5B H 0.5749 0.5603 0.2104 0.110 Uiso 0.50 1 calc PR . . N11 N 0.4813(3) 0.22552(16) 0.00869(14) 0.0585(10) Uani 1 1 d . . . C11 C 0.5799(5) 0.2529(3) 0.0225(3) 0.0915(19) Uani 1 1 d . . . H11A H 0.6353 0.2298 0.0295 0.137 Uiso 1 1 calc R . . H11B H 0.5731 0.2727 0.0480 0.137 Uiso 1 1 calc R . . H11C H 0.5944 0.2738 -0.0013 0.137 Uiso 1 1 calc R . . C12 C 0.4497(7) 0.1980(3) 0.0469(3) 0.112(2) Uani 1 1 d . . . H12A H 0.5017 0.1741 0.0571 0.168 Uiso 1 1 calc R . . H12B H 0.3853 0.1815 0.0377 0.168 Uiso 1 1 calc R . . H12C H 0.4417 0.2206 0.0703 0.168 Uiso 1 1 calc R . . C13 C 0.3953(9) 0.2607(4) -0.0087(3) 0.149(3) Uani 1 1 d . . . H13A H 0.3861 0.2844 0.0138 0.223 Uiso 1 1 calc R . . H13B H 0.3324 0.2425 -0.0164 0.223 Uiso 1 1 calc R . . H13C H 0.4128 0.2773 -0.0344 0.223 Uiso 1 1 calc R . . C14 C 0.4976(6) 0.1892(3) -0.0260(3) 0.115(2) Uani 1 1 d . . . H14A H 0.5069 0.2063 -0.0527 0.172 Uiso 1 1 calc R . . H14B H 0.4386 0.1680 -0.0315 0.172 Uiso 1 1 calc R . . H14C H 0.5580 0.1699 -0.0162 0.172 Uiso 1 1 calc R . . O1W O 0.2756(3) 0.82740(16) 0.11544(14) 0.0814(12) Uani 1 1 d . . . O2W O 0.6118(3) 0.39052(17) 0.08674(14) 0.0846(12) Uani 1 1 d . . . O3W O 0.1559(3) 0.66000(18) 0.19858(16) 0.0874(13) Uani 1 1 d . . . O4W O 0.2593(3) 0.3099(2) 0.29416(15) 0.0928(15) Uani 1 1 d . . . O5W O 0.0066(3) 0.56957(17) 0.05340(16) 0.0910(14) Uani 1 1 d . . . O6W O 0.1104(4) 0.5940(2) 0.91469(18) 0.1101(19) Uani 1 1 d . . . O7W O 0.6768(3) 0.6925(2) 0.12346(19) 0.1098(17) Uani 1 1 d . . . O8W O 0.6453(5) 0.3975(3) 0.2299(3) 0.169(3) Uani 1 1 d . . . O9W O 0.2345(7) 0.3841(3) 0.9093(3) 0.181(3) Uani 1 1 d . . . O10W O 0.0566(8) 0.3602(5) 0.1319(4) 0.118(4) Uani 0.50 1 d P . . O11W O 0.0877(8) 0.4042(6) 0.1424(4) 0.131(4) Uani 0.50 1 d P . . O12W O 0.0165(7) 0.3941(4) 0.8565(4) 0.114(4) Uani 0.50 1 d P . . O13W O 0.5717(10) 0.8610(5) 0.2288(4) 0.131(4) Uani 0.50 1 d P . . O14W O 0.1687(15) 0.3969(8) 0.7811(7) 0.114(6) Uani 0.25 1 d P . . O15W O 0.6265(14) 0.4510(6) 0.1584(5) 0.165(6) Uani 0.50 1 d P . . O16W O 0.141(2) 0.5250(8) 0.8525(7) 0.140(9) Uani 0.25 1 d P . . O17W O 0.910(3) 0.4897(8) 0.8570(7) 0.168(12) Uani 0.25 1 d P . . O18W O 0.205(2) 0.4310(9) 0.2006(12) 0.216(12) Uani 0.25 1 d P . . 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 0.04380(15) 0.04134(15) 0.04191(15) 0.00146(13) 0.00496(12) -0.00103(13) Mo2 0.04265(15) 0.04259(16) 0.04381(16) 0.00365(13) 0.00532(13) -0.00219(13) Mo3 0.03882(14) 0.04087(15) 0.04500(16) 0.00212(13) 0.00162(12) -0.00515(12) Mo4 0.03829(14) 0.03984(15) 0.04075(14) -0.00105(12) -0.00111(12) -0.00408(12) Mo5 0.03875(14) 0.04032(15) 0.04113(15) -0.00214(12) -0.00236(12) -0.00197(12) Mo6 0.04278(15) 0.04297(16) 0.04185(15) -0.00456(13) -0.00415(13) -0.00103(13) Mo7 0.05265(18) 0.05001(18) 0.04022(16) -0.00254(14) -0.00953(14) 0.00143(15) S1 0.0434(4) 0.0548(5) 0.0492(5) 0.0061(4) 0.0101(4) 0.0009(4) S2 0.0463(5) 0.0607(6) 0.0484(5) 0.0069(4) 0.0101(4) 0.0022(4) S3 0.0385(4) 0.0513(5) 0.0542(5) 0.0032(4) 0.0044(4) -0.0043(4) S4 0.0417(4) 0.0444(5) 0.0566(5) 0.0061(4) 0.0093(4) -0.0005(4) S5 0.0399(4) 0.0564(5) 0.0480(5) -0.0085(4) -0.0008(4) -0.0007(4) S6 0.0400(4) 0.0484(5) 0.0525(5) -0.0071(4) -0.0008(4) -0.0040(4) S7 0.0472(5) 0.0822(8) 0.0443(5) 0.0079(5) -0.0062(4) -0.0087(5) O1 0.074(2) 0.0471(16) 0.067(2) -0.0069(15) 0.0006(17) -0.0029(15) O2 0.0619(17) 0.0543(16) 0.0477(15) -0.0018(13) 0.0027(13) -0.0060(14) O3 0.0564(16) 0.0477(15) 0.0629(18) -0.0104(14) 0.0015(14) -0.0100(13) O4 0.0644(18) 0.0582(18) 0.0457(15) -0.0017(13) -0.0045(14) -0.0030(15) O5 0.0553(16) 0.0493(15) 0.0476(15) 0.0024(12) -0.0030(13) -0.0019(13) O6 0.0680(19) 0.0416(14) 0.0633(18) -0.0037(14) 0.0002(15) -0.0006(14) O7 0.094(3) 0.0556(19) 0.064(2) 0.0056(16) -0.0155(19) 0.0058(19) O8 0.0436(14) 0.0652(18) 0.0471(15) 0.0033(13) 0.0007(12) -0.0032(13) O9 0.0459(14) 0.0522(16) 0.0572(16) 0.0101(13) 0.0081(12) 0.0035(12) O10 0.0431(13) 0.0524(15) 0.0590(16) 0.0144(13) 0.0087(12) 0.0000(12) O11 0.0397(12) 0.0434(13) 0.0483(14) -0.0022(11) -0.0048(11) -0.0014(11) O12 0.0419(12) 0.0411(13) 0.0449(13) 0.0006(11) 0.0057(10) -0.0042(11) O13 0.0518(15) 0.075(2) 0.0409(14) -0.0117(14) -0.0028(12) -0.0030(15) O14 0.0474(15) 0.078(2) 0.0477(15) -0.0123(15) -0.0070(13) -0.0036(15) O15 0.056(2) 0.068(3) 0.067(3) 0.000 0.006(2) 0.000 O16 0.080(2) 0.0503(17) 0.0600(19) 0.0020(15) 0.0025(17) -0.0025(16) O17 0.0553(16) 0.0476(15) 0.0535(16) 0.0075(13) -0.0063(13) -0.0057(13) O18 0.0401(12) 0.0452(14) 0.0442(13) -0.0047(11) -0.0012(10) -0.0040(11) C1 0.049(2) 0.063(2) 0.0400(18) 0.0059(18) -0.0034(16) -0.0055(19) C2 0.160(6) 0.070(3) 0.067(3) 0.003(3) -0.050(4) -0.026(4) C3 0.131(5) 0.099(4) 0.103(4) -0.007(3) 0.004(4) -0.007(4) C4 0.179(7) 0.167(7) 0.094(4) -0.003(4) -0.005(4) 0.048(6) C5 0.072(3) 0.087(4) 0.111(5) -0.010(3) -0.001(3) -0.029(3) N11 0.0447(17) 0.058(2) 0.073(2) -0.0111(19) 0.0099(17) -0.0040(16) C11 0.072(3) 0.087(4) 0.111(5) -0.010(3) -0.001(3) -0.029(3) C12 0.131(5) 0.099(4) 0.103(4) -0.007(3) 0.004(4) -0.007(4) C13 0.179(7) 0.167(7) 0.094(4) -0.003(4) -0.005(4) 0.048(6) C14 0.092(4) 0.130(5) 0.131(5) -0.082(4) 0.046(4) -0.032(4) O1W 0.086(3) 0.083(3) 0.077(2) 0.000(2) 0.016(2) 0.016(2) O2W 0.0592(19) 0.111(3) 0.084(2) 0.044(2) 0.0096(18) -0.002(2) O3W 0.067(2) 0.091(3) 0.108(3) -0.019(2) 0.026(2) 0.002(2) O4W 0.064(2) 0.135(4) 0.080(3) -0.011(3) 0.012(2) -0.006(3) O5W 0.0524(18) 0.100(3) 0.122(3) -0.044(3) 0.017(2) -0.0209(19) O6W 0.107(4) 0.113(4) 0.102(4) 0.020(3) -0.017(3) -0.003(3) O7W 0.072(2) 0.128(4) 0.133(4) -0.036(3) 0.028(3) -0.045(2) O8W 0.144(5) 0.104(4) 0.279(9) 0.008(5) 0.095(5) -0.009(4) O9W 0.219(8) 0.174(7) 0.156(6) -0.046(5) 0.045(6) 0.040(6) O10W 0.076(6) 0.144(9) 0.134(8) 0.059(7) 0.016(6) 0.011(6) O11W 0.094(6) 0.201(12) 0.108(7) 0.042(8) 0.049(5) 0.054(7) O12W 0.085(5) 0.125(8) 0.139(8) -0.038(7) 0.045(5) -0.031(6) O13W 0.151(9) 0.148(11) 0.106(7) 0.009(7) 0.055(7) 0.006(9) O14W 0.103(11) 0.122(14) 0.131(13) -0.064(11) 0.067(10) -0.040(10) O15W 0.222(15) 0.165(13) 0.111(9) -0.012(9) 0.030(10) 0.032(12) O16W 0.22(3) 0.101(12) 0.098(12) -0.060(10) 0.018(15) 0.029(16) O17W 0.37(4) 0.073(12) 0.084(11) -0.021(9) 0.098(16) 0.009(18) O18W 0.213(18) 0.093(15) 0.39(3) -0.078(18) 0.222(19) -0.039(15) _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 1.677(3) . ? Mo1 O8 2.106(3) . ? Mo1 O8 2.120(3) 2_655 ? Mo1 S2 2.3083(12) . ? Mo1 S1 2.3212(11) . ? Mo1 Mo2 2.8284(5) . ? Mo2 O2 1.679(3) . ? Mo2 O10 2.062(3) . ? Mo2 O9 2.092(3) . ? Mo2 S2 2.3130(11) . ? Mo2 S1 2.3271(11) . ? Mo2 O16 2.461(3) . ? Mo3 O3 1.681(3) . ? Mo3 O10 2.066(3) . ? Mo3 O9 2.077(3) . ? Mo3 S4 2.3270(11) . ? Mo3 S3 2.3343(11) . ? Mo3 O17 2.413(3) . ? Mo3 Mo4 2.8240(5) . ? Mo4 O4 1.686(3) . ? Mo4 O11 2.100(3) . ? Mo4 O12 2.130(3) . ? Mo4 O18 2.302(3) . ? Mo4 S4 2.3200(11) . ? Mo4 S3 2.3243(11) . ? Mo5 O5 1.670(3) . ? Mo5 O11 2.093(3) . ? Mo5 O12 2.118(3) . ? Mo5 S5 2.3095(11) . ? Mo5 S6 2.3234(10) . ? Mo5 O18 2.465(3) . ? Mo5 Mo6 2.8164(5) . ? Mo6 O6 1.679(3) . ? Mo6 O13 2.057(3) . ? Mo6 O14 2.062(3) . ? Mo6 S6 2.3030(12) . ? Mo6 S5 2.3054(11) . ? Mo7 O7 1.664(4) . ? Mo7 O14 2.050(3) . ? Mo7 O13 2.064(3) . ? Mo7 S7 2.3006(12) . ? Mo7 S7 2.3110(13) 2_655 ? Mo7 Mo7 2.8069(7) 2_655 ? S7 Mo7 2.3110(13) 2_655 ? O8 Mo1 2.120(3) 2_655 ? O17 C1 1.257(6) . ? O18 C1 1.268(5) . ? C1 C2 1.501(7) . ? C2 C3 1.481(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.557(10) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.592(10) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4A' 0.9700 . ? C4 H4B' 0.9700 . ? C5 C4 1.462(10) 2_655 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? N11 C14 1.482(8) . ? N11 C12 1.490(10) . ? N11 C11 1.495(7) . ? N11 C13 1.513(11) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? O10W O11W 1.287(18) . ? 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 O8 99.19(16) . . ? O1 Mo1 O8 100.70(15) . 2_655 ? O8 Mo1 O8 72.13(14) . 2_655 ? O1 Mo1 S2 103.05(14) . . ? O8 Mo1 S2 151.29(9) . . ? O8 Mo1 S2 85.99(9) 2_655 . ? O1 Mo1 S1 103.53(13) . . ? O8 Mo1 S1 88.56(9) . . ? O8 Mo1 S1 151.10(9) 2_655 . ? S2 Mo1 S1 103.46(4) . . ? O1 Mo1 Mo2 101.33(12) . . ? O8 Mo1 Mo2 139.31(9) . . ? O8 Mo1 Mo2 136.23(9) 2_655 . ? S2 Mo1 Mo2 52.34(3) . . ? S1 Mo1 Mo2 52.61(3) . . ? O2 Mo2 O10 99.67(14) . . ? O2 Mo2 O9 96.84(14) . . ? O10 Mo2 O9 69.93(12) . . ? O2 Mo2 S2 101.81(12) . . ? O10 Mo2 S2 87.06(8) . . ? O9 Mo2 S2 152.52(9) . . ? O2 Mo2 S1 101.38(12) . . ? O10 Mo2 S1 154.10(10) . . ? O9 Mo2 S1 92.64(9) . . ? S2 Mo2 S1 103.13(4) . . ? O2 Mo2 O16 172.05(14) . . ? O10 Mo2 O16 75.58(12) . . ? O9 Mo2 O16 75.61(12) . . ? S2 Mo2 O16 84.46(9) . . ? S1 Mo2 O16 81.70(9) . . ? O2 Mo2 Mo1 98.47(11) . . ? O10 Mo2 Mo1 138.02(8) . . ? O9 Mo2 Mo1 144.00(9) . . ? S2 Mo2 Mo1 52.19(3) . . ? S1 Mo2 Mo1 52.43(3) . . ? O16 Mo2 Mo1 89.23(8) . . ? O3 Mo3 O10 99.48(14) . . ? O3 Mo3 O9 100.15(15) . . ? O10 Mo3 O9 70.14(12) . . ? O3 Mo3 S4 100.19(12) . . ? O10 Mo3 S4 88.73(9) . . ? O9 Mo3 S4 152.73(9) . . ? O3 Mo3 S3 100.53(12) . . ? O10 Mo3 S3 153.35(10) . . ? O9 Mo3 S3 89.10(9) . . ? S4 Mo3 S3 104.78(4) . . ? O3 Mo3 O17 177.01(14) . . ? O10 Mo3 O17 78.30(11) . . ? O9 Mo3 O17 77.25(11) . . ? S4 Mo3 O17 81.83(8) . . ? S3 Mo3 O17 80.99(8) . . ? O3 Mo3 Mo4 103.21(11) . . ? O10 Mo3 Mo4 137.66(8) . . ? O9 Mo3 Mo4 137.87(9) . . ? S4 Mo3 Mo4 52.46(3) . . ? S3 Mo3 Mo4 52.52(3) . . ? O17 Mo3 Mo4 79.77(7) . . ? O4 Mo4 O11 98.46(14) . . ? O4 Mo4 O12 100.61(14) . . ? O11 Mo4 O12 70.13(11) . . ? O4 Mo4 O18 168.90(14) . . ? O11 Mo4 O18 72.31(10) . . ? O12 Mo4 O18 70.76(10) . . ? O4 Mo4 S4 101.84(12) . . ? O11 Mo4 S4 151.90(8) . . ? O12 Mo4 S4 87.09(8) . . ? O18 Mo4 S4 85.01(7) . . ? O4 Mo4 S3 101.79(12) . . ? O11 Mo4 S3 89.15(8) . . ? O12 Mo4 S3 151.42(8) . . ? O18 Mo4 S3 84.55(8) . . ? S4 Mo4 S3 105.33(4) . . ? O4 Mo4 Mo3 105.76(12) . . ? O11 Mo4 Mo3 137.96(8) . . ? O12 Mo4 Mo3 135.24(7) . . ? O18 Mo4 Mo3 85.34(7) . . ? S4 Mo4 Mo3 52.69(3) . . ? S3 Mo4 Mo3 52.85(3) . . ? O5 Mo5 O11 97.64(13) . . ? O5 Mo5 O12 99.02(13) . . ? O11 Mo5 O12 70.51(11) . . ? O5 Mo5 S5 103.95(12) . . ? O11 Mo5 S5 89.72(9) . . ? O12 Mo5 S5 151.49(8) . . ? O5 Mo5 S6 103.02(11) . . ? O11 Mo5 S6 153.03(8) . . ? O12 Mo5 S6 89.11(8) . . ? S5 Mo5 S6 101.75(4) . . ? O5 Mo5 O18 163.44(12) . . ? O11 Mo5 O18 69.09(10) . . ? O12 Mo5 O18 67.74(10) . . ? S5 Mo5 O18 86.35(7) . . ? S6 Mo5 O18 87.17(7) . . ? O5 Mo5 Mo6 97.68(10) . . ? O11 Mo5 Mo6 141.53(8) . . ? O12 Mo5 Mo6 140.46(7) . . ? S5 Mo5 Mo6 52.32(3) . . ? S6 Mo5 Mo6 52.17(3) . . ? O18 Mo5 Mo6 98.88(6) . . ? O6 Mo6 O13 107.56(16) . . ? O6 Mo6 O14 105.37(15) . . ? O13 Mo6 O14 68.72(13) . . ? O6 Mo6 S6 106.45(13) . . ? O13 Mo6 S6 141.63(10) . . ? O14 Mo6 S6 85.58(10) . . ? O6 Mo6 S5 105.62(12) . . ? O13 Mo6 S5 84.94(9) . . ? O14 Mo6 S5 144.09(10) . . ? S6 Mo6 S5 102.50(4) . . ? O6 Mo6 Mo5 101.98(11) . . ? O13 Mo6 Mo5 133.47(10) . . ? O14 Mo6 Mo5 135.34(10) . . ? S6 Mo6 Mo5 52.83(3) . . ? S5 Mo6 Mo5 52.46(3) . . ? O7 Mo7 O14 105.38(17) . . ? O7 Mo7 O13 106.70(16) . . ? O14 Mo7 O13 68.83(13) . . ? O7 Mo7 S7 106.22(15) . . ? O14 Mo7 S7 86.14(9) . . ? O13 Mo7 S7 142.81(10) . . ? O7 Mo7 S7 106.67(15) . 2_655 ? O14 Mo7 S7 143.23(11) . 2_655 ? O13 Mo7 S7 85.00(10) . 2_655 ? S7 Mo7 S7 101.64(4) . 2_655 ? O7 Mo7 Mo7 101.09(13) . 2_655 ? O14 Mo7 Mo7 136.01(9) . 2_655 ? O13 Mo7 Mo7 134.42(9) . 2_655 ? S7 Mo7 Mo7 52.68(3) . 2_655 ? S7 Mo7 Mo7 52.34(3) 2_655 2_655 ? Mo1 S1 Mo2 74.96(3) . . ? Mo1 S2 Mo2 75.47(4) . . ? Mo4 S3 Mo3 74.63(3) . . ? Mo4 S4 Mo3 74.85(3) . . ? Mo6 S5 Mo5 75.22(3) . . ? Mo6 S6 Mo5 75.00(3) . . ? Mo7 S7 Mo7 74.99(4) . 2_655 ? Mo1 O8 Mo1 105.13(13) . 2_655 ? Mo3 O9 Mo2 107.43(14) . . ? Mo2 O10 Mo3 108.98(13) . . ? Mo5 O11 Mo4 102.54(11) . . ? Mo5 O12 Mo4 100.70(11) . . ? Mo6 O13 Mo7 106.83(15) . . ? Mo7 O14 Mo6 107.19(15) . . ? C1 O17 Mo3 127.2(3) . . ? C1 O18 Mo4 125.6(3) . . ? C1 O18 Mo5 147.8(3) . . ? Mo4 O18 Mo5 86.59(9) . . ? O17 C1 O18 122.1(4) . . ? O17 C1 C2 121.0(4) . . ? O18 C1 C2 116.9(4) . . ? C3 C2 C1 117.3(5) . . ? C3 C2 H2A 108.0 . . ? C1 C2 H2A 108.0 . . ? C3 C2 H2B 108.0 . . ? C1 C2 H2B 108.0 . . ? H2A C2 H2B 107.2 . . ? C2 C3 C4 105.0(6) . . ? C2 C3 H3A 110.7 . . ? C4 C3 H3A 110.7 . . ? C2 C3 H3B 110.7 . . ? C4 C3 H3B 110.7 . . ? H3A C3 H3B 108.8 . . ? C3 C4 C5 94.7(7) . . ? C3 C4 H4A 112.8 . . ? C5 C4 H4A 112.8 . . ? C3 C4 H4B 112.8 . . ? C5 C4 H4B 112.8 . . ? H4A C4 H4B 110.3 . . ? C4 C5 C4 108.7(8) 2_655 . ? C4 C5 H5A 109.9 2_655 . ? C4 C5 H5A 109.9 . . ? C4 C5 H5B 109.9 2_655 . ? C4 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? C14 N11 C12 107.9(5) . . ? C14 N11 C11 109.1(5) . . ? C12 N11 C11 110.5(5) . . ? C14 N11 C13 110.0(6) . . ? C12 N11 C13 108.5(6) . . ? C11 N11 C13 110.9(6) . . ? N11 C11 H11A 109.5 . . ? N11 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N11 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N11 C12 H12A 109.5 . . ? N11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N11 C13 H13A 109.5 . . ? N11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N11 C14 H14A 109.5 . . ? N11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.08 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.937 _refine_diff_density_min -1.699 _refine_diff_density_rms 0.318 #===END