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#\#CIF_1.0 ################################################################################ # # # This CIF is a part of the B-IncStrDB # # (Bilbao Incommensurate Structures Database) # # http://www.cryst.ehu.eus/bincstrdb/ # # # # Please note that the structure of the CIF file may differ from the one # # deposited, as it may have been modified to comply with the standard. The # # file has been validated against official dictionaries as well as local # # dictionaries including non-standard data names used by SHELXL (Sheldrick, # # G. M. (2008). Acta Cryst. A 64, 112-122) and JANA (Petricek, V., Dusek, M. # # and Palatinus, L. (2014), Z. Kristallogr. 229, 345-352). # # # # For comments and/or criticisms, please e-mail to administrador-bcs@ehu.es # # # ################################################################################ ############################################################################## # # # This CIF contains the data in a paper accepted for publication in Acta # # Crystallographica Section B. It has been peer reviewed under the auspices # # of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary may be obtained from # # ftp://ftp.iucr.org/pub/cif_core.dic. The current version number is 2.1. # # # # Software is freely available for graphical display of the structure(s) in # # this CIF. For information consult the CIF home page http://www.iucr.org/ # # cif/home.html # # # # Copyright International Union of Crystallography # # # ############################################################################## data_global _audit_creation_method 'Jana2000 Version : 26/01/2006' _journal_date_recd_electronic 2006-04-24 _journal_date_accepted 2006-07-04 _journal_name_full 'Acta Crystallographica, Section B' _journal_year 2006 _journal_volume 62 _journal_issue 2 _journal_page_first 790 _journal_page_last 797 _journal_paper_doi https://doi.org/10.1107/S0108768106025791 _journal_paper_category FA _journal_coeditor_code SN5039 _publ_contact_author_name 'Evain, Michel' _publ_contact_author_address ;Laboratoire de Chimie des Solides IMN UMR 6502 CNRS - Universite de Nantes 2 rue de la Houssiniere BP 32229 44322 Nantes CEDEX 3 France ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_section_title ;Commensurate (C~6~H~14~N~2~)~2~[Mo~8~O~26~]⋅4H~2~O and incommensurate (C~6~H~14~N~2~)~2~[Mo~8~O~26~]⋅4.66H~2~O: a structural versatility linked to solvent content ; loop_ _publ_author_name _publ_author_address 'Evain, Michel' ;Laboratoire de Chimie des Solides IMN UMR 6502 CNRS - Universite de Nantes 2 rue de la Houssiniere BP 32229 44322 Nantes CEDEX 3 France ; 'Petricek, Vaclav' ;Institute of Physics Academy of Sciences of the Czech Republic Na Slovance 2 182 21 Praha 8 Czech Republic ; 'Coue, Violaine' ;Laboratoire de Chimie des Solides IMN UMR 6502 CNRS - Universite de Nantes 2 rue de la Houssiniere BP 32229 44322 Nantes CEDEX 3 France ; 'Dessapt, Remi' ;Laboratoire de Chimie des Solides IMN UMR 6502 CNRS - Universite de Nantes 2 rue de la Houssiniere BP 32229 44322 Nantes CEDEX 3 France ; 'Bujoli-Doeuff, Martine' ;Laboratoire de Chimie des Solides IMN UMR 6502 CNRS - Universite de Nantes 2 rue de la Houssiniere BP 32229 44322 Nantes CEDEX 3 France ; 'Jobic, Stephane' ;Laboratoire de Chimie des Solides IMN UMR 6502 CNRS - Universite de Nantes 2 rue de la Houssiniere BP 32229 44322 Nantes CEDEX 3 France ; data_I _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H36 Mo8 N4 O30' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac '(C6 H14 N2)2 [Mo8 O26], 4H2 O' _chemical_formula_weight 1483.9 _chemical_melting_point ? _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x,-y,-z _cell_length_a 12.3378(15) _cell_length_b 14.417(2) _cell_length_c 16.1439(16) _cell_angle_alpha 100.927(9) _cell_angle_beta 106.487(8) _cell_angle_gamma 104.110(10) _cell_volume 2565.0(6) _cell_formula_units_Z 3 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature ? _exptl_crystal_type_of_structure cryst _exptl_crystal_description 'elongated block' _exptl_crystal_colour 'colourless' _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.8811 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 2.946 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details '(Jana2000; Petricek, Dusek & Palatinus, 2000)' _exptl_absorpt_correction_T_min 0.595 _exptl_absorpt_correction_T_max 0.833 _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Nonius CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 90290 _diffrn_reflns_av_R_equivalents 0.0681 _diffrn_reflns_av_unetI/netI 0.0485 _diffrn_reflns_theta_min 6.41 _diffrn_reflns_theta_max 35.00 _diffrn_reflns_theta_full 35.00 _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full 0.97 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_reduction_process ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _reflns_number_total 21895 _reflns_number_gt 14316 _reflns_threshold_expression 'I>2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.1146 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_gt 0.1076 _refine_ls_wR_factor_ref 0.1351 _refine_ls_goodness_of_fit_ref 1.43 _refine_ls_restrained_S_all ? _refine_ls_number_reflns 21895 _refine_ls_number_parameters 730 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(I)+0.001936I^2^)' _refine_ls_shift/su_max 0.0009 _refine_ls_shift/su_mean 0.0000 _refine_diff_density_max 1.61 _refine_diff_density_min -1.89 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo -1.683 0.686 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' H 0.000 0.000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement '(Jana2000; Petricek and Dusek, 2000)' _computing_molecular_graphics ? _computing_publication_material '(Jana2000; Petricek and Dusek, 2000)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo1 0.25888(4) 0.37951(3) -0.02610(3) 0.01868(14) Uani d . 1 . . Mo Mo2 0.47524(3) 0.44973(3) 0.17692(3) 0.01540(13) Uani d . 1 . . Mo Mo3 0.78573(4) 0.39209(3) 0.20671(3) 0.01813(14) Uani d . 1 . . Mo Mo4 0.57152(4) 0.35669(3) 0.02056(3) 0.01616(13) Uani d . 1 . . Mo Mo5 0.19472(4) 0.28345(3) 0.12704(3) 0.01999(14) Uani d . 1 . . Mo Mo6 0.40766(4) 0.30695(3) 0.31313(3) 0.01689(13) Uani d . 1 . . Mo Mo7 0.73264(4) 0.29683(3) 0.36259(3) 0.01807(13) Uani d . 1 . . Mo Mo8 0.50910(3) 0.21841(3) 0.16045(3) 0.01450(12) Uani d . 1 . . Mo Mo9 0.25284(4) 0.03970(3) 0.30053(3) 0.01699(13) Uani d . 1 . . Mo Mo10 0.47035(3) 0.11159(3) 0.50438(3) 0.01507(13) Uani d . 1 . . Mo Mo11 0.79453(4) 0.07729(3) 0.55027(3) 0.01802(14) Uani d . 1 . . Mo Mo12 0.58281(3) 0.03153(3) 0.35728(3) 0.01555(13) Uani d . 1 . . O O1 0.1439(3) 0.4283(3) -0.0297(3) 0.0288(15) Uani d . 1 . . O O2 0.3126(3) 0.4319(2) 0.1275(2) 0.0197(12) Uani d . 1 . . O O3 0.2422(4) 0.3269(3) -0.1334(3) 0.0329(16) Uani d . 1 . . O O4 0.2041(3) 0.2636(2) 0.0066(2) 0.0239(13) Uani d . 1 . . O O5 0.4323(3) 0.3823(2) 0.0356(2) 0.0190(12) Uani d . 1 . . O O6 0.6392(3) 0.4761(3) 0.0140(2) 0.0248(14) Uani d . 1 . . O O7 0.5415(3) 0.5700(2) 0.1852(2) 0.0244(13) Uani d . 1 . . O O8 0.4883(3) 0.4512(2) 0.2886(2) 0.0216(12) Uani d . 1 . . O O9 0.3831(3) 0.2770(2) 0.1667(2) 0.0172(11) Uani d . 1 . . O O10 0.5968(3) 0.3900(2) 0.1659(2) 0.0168(11) Uani d . 1 . . O O11 0.7750(3) 0.4135(2) 0.3246(2) 0.0207(12) Uani d . 1 . . O O12 0.6717(3) 0.2411(2) 0.2095(2) 0.0178(11) Uani d . 1 . . O O13 0.9058(3) 0.3505(3) 0.2219(3) 0.0279(14) Uani d . 1 . . O O14 0.8396(3) 0.5127(3) 0.2103(3) 0.0300(15) Uani d . 1 . . O O15 0.7127(3) 0.3312(2) 0.0753(2) 0.0200(12) Uani d . 1 . . O O16 0.5255(3) 0.2839(3) -0.0866(2) 0.0278(14) Uani d . 1 . . O O17 0.4933(3) 0.2145(2) 0.0475(2) 0.0204(12) Uani d . 1 . . O O18 0.0803(3) 0.3319(3) 0.1124(3) 0.0320(16) Uani d . 1 . . O O19 0.2666(3) 0.3344(2) 0.2581(2) 0.0220(13) Uani d . 1 . . O O20 0.1304(3) 0.1619(3) 0.1169(3) 0.0302(15) Uani d . 1 . . O O21 0.4502(3) 0.3767(3) 0.4206(2) 0.0269(14) Uani d . 1 . . O O22 0.3380(3) 0.1833(2) 0.3152(2) 0.0225(13) Uani d . 1 . . O O23 0.5473(3) 0.2849(2) 0.2999(2) 0.0183(11) Uani d . 1 . . O O24 0.7375(4) 0.3517(3) 0.4661(2) 0.0318(15) Uani d . 1 . . O O25 0.6430(3) 0.1530(3) 0.3514(2) 0.0244(13) Uani d . 1 . . O O26 0.8596(3) 0.2659(3) 0.3768(3) 0.0326(16) Uani d . 1 . . O O27 0.4466(3) 0.0978(2) 0.1529(2) 0.0236(13) Uani d . 1 . . O O28 0.2440(3) -0.0133(3) 0.1952(2) 0.0284(14) Uani d . 1 . . O O29 0.1203(3) 0.0610(3) 0.2882(3) 0.0287(15) Uani d . 1 . . O O30 0.3059(3) 0.0801(2) 0.4507(2) 0.0181(11) Uani d . 1 . . O O31 0.4383(3) 0.0457(2) 0.3650(2) 0.0185(11) Uani d . 1 . . O O32 0.7852(3) 0.0859(2) 0.6684(2) 0.0212(12) Uani d . 1 . . O O33 0.5254(3) 0.2329(3) 0.5108(2) 0.0255(13) Uani d . 1 . . O O34 0.4806(3) 0.1136(2) 0.6158(2) 0.0200(12) Uani d . 1 . . O O35 0.6030(3) 0.0628(2) 0.5022(2) 0.0166(11) Uani d . 1 . . O O36 0.9235(3) 0.0487(3) 0.5637(3) 0.0313(16) Uani d . 1 . . O O37 0.8354(3) 0.2015(3) 0.5621(3) 0.0301(15) Uani d . 1 . . O O38 0.7321(3) 0.0195(2) 0.4192(2) 0.0199(12) Uani d . 1 . . O O39 0.5488(3) -0.0410(3) 0.2517(2) 0.0273(14) Uani d . 1 . . O O1w 0.6356(5) 0.1282(3) -0.0883(3) 0.049(2) Uani d . 1 . . O O2w 0.3364(6) 0.2032(4) 0.7346(4) 0.072(3) Uani d . 1 . . O O3w 0.9070(4) 0.0220(4) 0.3469(3) 0.058(3) Uani d . 1 . . O O4w 0.3259(5) 0.5541(4) 0.3805(4) 0.062(3) Uani d . 1 . . O O5w 0.0931(6) 0.4624(5) 0.3786(5) 0.095(3) Uani d . 1 . . O O6w 0.0438(9) 0.1717(8) 0.7667(7) 0.155(6) Uani d . 1 . . N N1 0.8624(4) 0.0250(4) 0.1750(3) 0.040(2) Uani d . 1 . . N N2 0.7548(4) 0.0513(3) 0.0324(3) 0.0333(19) Uani d . 1 . . N N3 0.1441(4) 0.3577(4) 0.4954(3) 0.038(2) Uani d . 1 . . N N4 0.2270(5) 0.2680(4) 0.6006(4) 0.041(2) Uani d . 1 . . N N5 0.1652(4) 0.7345(3) 0.2214(3) 0.0314(18) Uani d . 1 . . N N6 0.1766(4) 0.5803(4) 0.1333(3) 0.039(2) Uani d . 1 . . C C1 0.8958(6) -0.0270(4) 0.1009(4) 0.046(3) Uani d . 1 . . C C2 0.8160(6) -0.0218(5) 0.0127(4) 0.045(3) Uani d . 1 . . C C3 0.7329(7) -0.0151(7) 0.1538(6) 0.076(4) Uani d . 1 . . C C4 0.6688(6) 0.0134(5) 0.0734(5) 0.047(3) Uani d . 1 . . C C5 0.8963(5) 0.1333(4) 0.1830(4) 0.036(2) Uani d . 1 . . C C6 0.8431(6) 0.1467(4) 0.0923(4) 0.042(2) Uani d . 1 . . C C7 0.2757(6) 0.4069(5) 0.5393(5) 0.045(3) Uani d . 1 . . C C8 0.3254(6) 0.3368(5) 0.5856(5) 0.043(3) Uani d . 1 . . C C9 0.0873(6) 0.3610(4) 0.5656(4) 0.037(2) Uani d . 1 . . C C10 0.1576(7) 0.3253(5) 0.6393(5) 0.050(3) Uani d . 1 . . C C11 0.1189(6) 0.2522(5) 0.4454(5) 0.052(3) Uani d . 1 . . C C12 0.1450(6) 0.1953(5) 0.5127(5) 0.048(3) Uani d . 1 . . C C13 0.2889(6) 0.7334(5) 0.2532(5) 0.050(3) Uani d . 1 . . C C14 0.2968(6) 0.6371(5) 0.2002(5) 0.046(3) Uani d . 1 . . C C15 0.0833(6) 0.6484(4) 0.2338(5) 0.045(3) Uani d . 1 . . C C16 0.0915(6) 0.5531(4) 0.1800(4) 0.040(3) Uani d . 1 . . C C17 0.1283(6) 0.7324(5) 0.1261(4) 0.043(3) Uani d . 1 . . C C18 0.1367(6) 0.6377(5) 0.0712(5) 0.047(3) Uani d . 1 . . H H1 0.90068 0.014916 0.228745 0.0477 Uiso d . 1 . . H H2 0.713278 0.061415 -0.020427 0.04 Uiso d . 1 . . H H3 0.113319 0.390683 0.455632 0.0458 Uiso d . 1 . . H H4 0.259328 0.235369 0.640034 0.0492 Uiso d . 1 . . H H5 0.162046 0.792501 0.254619 0.0377 Uiso d . 1 . . H H6 0.179833 0.522834 0.099284 0.047 Uiso d . 1 . . H H7 0.883728 -0.096075 0.100705 0.0546 Uiso d . 1 . . H H8 0.978245 0.006566 0.1096 0.0546 Uiso d . 1 . . H H9 0.863931 -0.000335 -0.022679 0.0544 Uiso d . 1 . . H H10 0.757395 -0.086715 -0.019507 0.0544 Uiso d . 1 . . H H11 0.71248 0.012056 0.204867 0.0911 Uiso d . 1 . . H H12 0.709345 -0.087072 0.140614 0.0911 Uiso d . 1 . . H H13 0.606272 -0.0449 0.03058 0.0558 Uiso d . 1 . . H H14 0.636313 0.065062 0.092638 0.0558 Uiso d . 1 . . H H15 0.982426 0.160933 0.203266 0.0428 Uiso d . 1 . . H H16 0.865215 0.165845 0.224967 0.0428 Uiso d . 1 . . H H17 0.804073 0.197236 0.097674 0.0501 Uiso d . 1 . . H H18 0.905428 0.166639 0.067615 0.0501 Uiso d . 1 . . H H19 0.291447 0.468819 0.583578 0.0542 Uiso d . 1 . . H H20 0.31064 0.417828 0.493792 0.0542 Uiso d . 1 . . H H21 0.35691 0.299024 0.547422 0.0513 Uiso d . 1 . . H H22 0.386936 0.374826 0.643061 0.0513 Uiso d . 1 . . H H23 0.005762 0.316752 0.539593 0.0449 Uiso d . 1 . . H H24 0.090903 0.428932 0.590205 0.0449 Uiso d . 1 . . H H25 0.212324 0.382228 0.688631 0.0599 Uiso d . 1 . . H H26 0.103191 0.281913 0.659262 0.0599 Uiso d . 1 . . H H27 0.035518 0.224451 0.407506 0.0623 Uiso d . 1 . . H H28 0.170023 0.24934 0.409748 0.0623 Uiso d . 1 . . H H29 0.071375 0.160726 0.519416 0.0582 Uiso d . 1 . . H H30 0.183618 0.148654 0.493142 0.0582 Uiso d . 1 . . H H31 0.313096 0.736754 0.316669 0.0596 Uiso d . 1 . . H H32 0.340631 0.789987 0.244056 0.0596 Uiso d . 1 . . H H33 0.352708 0.652938 0.169147 0.0553 Uiso d . 1 . . H H34 0.320902 0.598268 0.240772 0.0553 Uiso d . 1 . . H H35 0.002365 0.650334 0.212039 0.0537 Uiso d . 1 . . H H36 0.107055 0.650639 0.297052 0.0537 Uiso d . 1 . . H H37 0.119845 0.515395 0.220375 0.0482 Uiso d . 1 . . H H38 0.013699 0.514085 0.135906 0.0482 Uiso d . 1 . . H H39 0.180382 0.790057 0.118523 0.0522 Uiso d . 1 . . H H40 0.046706 0.733304 0.105896 0.0522 Uiso d . 1 . . H H41 0.058756 0.598646 0.027298 0.0561 Uiso d . 1 . . H H42 0.194311 0.655116 0.041899 0.0561 Uiso d . 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Mo1 0.01580(18) 0.01817(18) 0.0225(2) 0.00485(14) 0.00681(16) 0.00696(15) Mo Mo2 0.01421(17) 0.01238(16) 0.02019(19) 0.00386(13) 0.00687(15) 0.00489(13) Mo Mo3 0.01457(18) 0.01746(18) 0.0230(2) 0.00302(14) 0.00833(16) 0.00697(15) Mo Mo4 0.01711(18) 0.01583(17) 0.01909(19) 0.00618(14) 0.00918(15) 0.00713(14) Mo Mo5 0.01552(18) 0.01765(18) 0.0279(2) 0.00319(14) 0.00980(17) 0.00805(15) Mo Mo6 0.01832(19) 0.01529(17) 0.02046(19) 0.00559(14) 0.01050(16) 0.00655(14) Mo Mo7 0.01560(18) 0.01834(18) 0.01871(19) 0.00269(14) 0.00569(15) 0.00551(14) Mo Mo8 0.01366(17) 0.01222(16) 0.01815(18) 0.00368(13) 0.00649(14) 0.00443(13) Mo Mo9 0.01405(17) 0.01775(18) 0.01901(19) 0.00330(13) 0.00595(15) 0.00667(14) Mo Mo10 0.01321(17) 0.01381(17) 0.01882(18) 0.00385(13) 0.00652(14) 0.00507(13) Mo Mo11 0.01324(17) 0.01954(18) 0.0219(2) 0.00333(13) 0.00701(15) 0.00811(15) Mo Mo12 0.01403(17) 0.01682(17) 0.01800(18) 0.00478(13) 0.00778(14) 0.00653(14) Mo O1 0.0243(19) 0.030(2) 0.038(2) 0.0123(15) 0.0139(17) 0.0144(17) O O2 0.0179(16) 0.0142(15) 0.0280(18) 0.0048(12) 0.0090(14) 0.0066(13) O O3 0.036(2) 0.033(2) 0.028(2) 0.0089(17) 0.0106(18) 0.0074(16) O O4 0.0244(18) 0.0191(16) 0.0239(18) 0.0027(13) 0.0079(15) 0.0026(13) O O5 0.0167(16) 0.0207(16) 0.0222(17) 0.0072(12) 0.0079(13) 0.0080(13) O O6 0.0213(18) 0.0234(18) 0.035(2) 0.0073(14) 0.0117(16) 0.0154(15) O O7 0.0240(18) 0.0168(16) 0.033(2) 0.0058(13) 0.0105(16) 0.0093(14) O O8 0.0248(18) 0.0181(16) 0.0225(17) 0.0048(13) 0.0105(15) 0.0061(13) O O9 0.0147(15) 0.0169(15) 0.0225(16) 0.0066(12) 0.0087(13) 0.0057(12) O O10 0.0139(15) 0.0181(15) 0.0210(16) 0.0064(12) 0.0078(13) 0.0073(12) O O11 0.0217(17) 0.0152(15) 0.0221(17) 0.0011(12) 0.0079(14) 0.0039(12) O O12 0.0140(15) 0.0163(15) 0.0251(17) 0.0061(12) 0.0088(13) 0.0060(12) O O13 0.0202(18) 0.034(2) 0.032(2) 0.0101(15) 0.0101(16) 0.0090(16) O O14 0.028(2) 0.0222(18) 0.040(2) 0.0017(15) 0.0152(18) 0.0124(16) O O15 0.0190(16) 0.0210(16) 0.0249(17) 0.0077(13) 0.0120(14) 0.0090(13) O O16 0.033(2) 0.0287(19) 0.0232(18) 0.0095(16) 0.0124(16) 0.0080(15) O O17 0.0220(17) 0.0180(16) 0.0225(17) 0.0057(13) 0.0102(14) 0.0054(13) O O18 0.0228(19) 0.033(2) 0.045(2) 0.0123(16) 0.0143(18) 0.0128(18) O O19 0.0218(17) 0.0228(17) 0.0286(18) 0.0104(14) 0.0155(15) 0.0089(14) O O20 0.030(2) 0.0213(18) 0.041(2) 0.0022(15) 0.0191(18) 0.0095(16) O O21 0.035(2) 0.0249(18) 0.0235(18) 0.0109(15) 0.0135(16) 0.0047(14) O O22 0.0206(17) 0.0202(16) 0.0308(19) 0.0060(13) 0.0119(15) 0.0125(14) O O23 0.0159(15) 0.0200(16) 0.0191(16) 0.0043(12) 0.0068(13) 0.0062(12) O O24 0.037(2) 0.030(2) 0.0228(19) 0.0029(17) 0.0115(17) 0.0024(15) O O25 0.0198(17) 0.0237(17) 0.035(2) 0.0066(14) 0.0119(15) 0.0169(15) O O26 0.0217(19) 0.039(2) 0.040(2) 0.0125(17) 0.0084(17) 0.0175(18) O O27 0.0228(18) 0.0166(15) 0.0284(19) 0.0018(13) 0.0087(15) 0.0056(13) O O28 0.033(2) 0.0264(18) 0.0224(18) 0.0041(15) 0.0107(16) 0.0048(14) O O29 0.0204(18) 0.034(2) 0.041(2) 0.0139(16) 0.0131(17) 0.0200(17) O O30 0.0163(15) 0.0228(16) 0.0178(16) 0.0084(13) 0.0073(13) 0.0068(12) O O31 0.0154(15) 0.0203(16) 0.0203(16) 0.0052(12) 0.0068(13) 0.0061(12) O O32 0.0226(17) 0.0164(15) 0.0239(17) 0.0029(13) 0.0097(14) 0.0062(13) O O33 0.0245(18) 0.0197(16) 0.032(2) 0.0037(14) 0.0108(16) 0.0102(14) O O34 0.0170(16) 0.0217(16) 0.0181(16) 0.0021(12) 0.0071(13) 0.0024(12) O O35 0.0151(15) 0.0177(15) 0.0163(15) 0.0040(11) 0.0056(12) 0.0043(12) O O36 0.0201(18) 0.047(2) 0.036(2) 0.0154(17) 0.0142(17) 0.0196(18) O O37 0.031(2) 0.0240(18) 0.032(2) 0.0004(15) 0.0105(17) 0.0108(15) O O38 0.0172(16) 0.0245(17) 0.0220(17) 0.0085(13) 0.0107(14) 0.0072(13) O O39 0.029(2) 0.0315(19) 0.0225(18) 0.0103(16) 0.0096(16) 0.0070(15) O O1w 0.059(3) 0.035(2) 0.042(3) 0.024(2) -0.003(2) 0.001(2) O O2w 0.084(4) 0.047(3) 0.062(4) 0.032(3) -0.006(3) -0.001(3) O O3w 0.045(3) 0.110(4) 0.041(3) 0.044(3) 0.022(2) 0.032(3) O O4w 0.071(4) 0.048(3) 0.063(4) 0.018(3) 0.027(3) 0.003(3) O O5w 0.070(4) 0.085(5) 0.088(5) -0.011(3) -0.018(4) 0.045(4) O O6w 0.127(8) 0.147(9) 0.149(9) 0.028(7) 0.018(7) 0.010(7) O N1 0.036(3) 0.051(3) 0.029(3) 0.007(2) 0.006(2) 0.021(2) N N2 0.028(2) 0.035(3) 0.033(3) 0.014(2) 0.003(2) 0.008(2) N N3 0.031(3) 0.045(3) 0.038(3) 0.013(2) 0.011(2) 0.009(2) N N4 0.040(3) 0.037(3) 0.051(3) 0.015(2) 0.017(3) 0.015(2) N N5 0.033(3) 0.018(2) 0.037(3) 0.0040(17) 0.012(2) -0.0021(18) N N6 0.039(3) 0.028(2) 0.047(3) 0.006(2) 0.024(3) -0.005(2) N C1 0.043(4) 0.030(3) 0.049(4) 0.019(3) -0.003(3) -0.003(3) C C2 0.047(4) 0.051(4) 0.036(3) 0.026(3) 0.015(3) -0.004(3) C C3 0.041(5) 0.111(8) 0.061(5) -0.011(5) 0.021(4) 0.030(5) C C4 0.021(3) 0.053(4) 0.058(4) 0.005(3) 0.015(3) 0.005(3) C C5 0.031(3) 0.029(3) 0.036(3) 0.008(2) 0.006(3) -0.003(2) C C6 0.035(3) 0.028(3) 0.049(4) 0.005(2) 0.000(3) 0.008(3) C C7 0.033(3) 0.039(4) 0.067(5) 0.009(3) 0.025(3) 0.013(3) C C8 0.027(3) 0.038(3) 0.051(4) 0.007(3) 0.004(3) 0.004(3) C C9 0.033(3) 0.034(3) 0.042(3) 0.011(2) 0.017(3) -0.003(3) C C10 0.062(5) 0.058(5) 0.048(4) 0.034(4) 0.032(4) 0.017(3) C C11 0.040(4) 0.047(4) 0.049(4) 0.013(3) 0.005(3) -0.015(3) C C12 0.033(3) 0.026(3) 0.076(5) 0.003(2) 0.019(3) -0.003(3) C C13 0.029(3) 0.042(4) 0.054(4) 0.002(3) -0.004(3) -0.002(3) C C14 0.037(4) 0.051(4) 0.060(5) 0.020(3) 0.024(3) 0.017(3) C C15 0.051(4) 0.035(3) 0.051(4) 0.005(3) 0.035(4) 0.002(3) C C16 0.046(4) 0.024(3) 0.048(4) 0.000(2) 0.028(3) 0.001(2) C C17 0.041(4) 0.042(4) 0.042(4) 0.005(3) 0.012(3) 0.014(3) C C18 0.039(4) 0.049(4) 0.040(4) 0.003(3) 0.018(3) -0.006(3) C loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Mo1 O1 . . 1.722(5) yes Mo1 O2 . . 2.295(4) yes Mo1 O3 . . 1.685(4) yes Mo1 O4 . . 1.874(4) yes Mo1 O5 . . 2.075(3) yes Mo1 O6 . 2_665 2.094(4) yes Mo2 O2 . . 1.869(3) yes Mo2 O5 . . 2.156(3) yes Mo2 O7 . . 1.689(3) yes Mo2 O8 . . 1.760(4) yes Mo2 O9 . . 2.425(3) yes Mo2 O10 . . 1.936(4) yes Mo3 O10 . . 2.226(3) yes Mo3 O11 . . 1.916(4) yes Mo3 O12 . . 2.303(3) yes Mo3 O13 . . 1.702(4) yes Mo3 O14 . . 1.686(4) yes Mo3 O15 . . 1.976(3) yes Mo4 O5 . . 1.913(4) yes Mo4 O6 . . 1.758(4) yes Mo4 O10 . . 2.218(4) yes Mo4 O15 . . 1.874(4) yes Mo4 O16 . . 1.697(3) yes Mo4 O17 . . 2.221(4) yes Mo5 O2 . . 2.273(3) yes Mo5 O4 . . 1.952(4) yes Mo5 O9 . . 2.259(4) yes Mo5 O18 . . 1.700(5) yes Mo5 O19 . . 1.957(3) yes Mo5 O20 . . 1.694(4) yes Mo6 O8 . . 2.236(4) yes Mo6 O9 . . 2.238(4) yes Mo6 O19 . . 1.888(4) yes Mo6 O21 . . 1.691(4) yes Mo6 O22 . . 1.792(4) yes Mo6 O23 . . 1.888(4) yes Mo7 O11 . . 1.904(4) yes Mo7 O12 . . 2.284(3) yes Mo7 O23 . . 2.170(3) yes Mo7 O24 . . 1.685(4) yes Mo7 O25 . . 2.045(4) yes Mo7 O26 . . 1.697(5) yes Mo8 O9 . . 1.959(4) yes Mo8 O10 . . 2.419(3) yes Mo8 O12 . . 1.854(3) yes Mo8 O17 . . 1.767(4) yes Mo8 O23 . . 2.138(3) yes Mo8 O27 . . 1.687(3) yes Mo9 O22 . . 2.014(3) yes Mo9 O28 . . 1.687(4) yes Mo9 O29 . . 1.701(4) yes Mo9 O30 . . 2.241(3) yes Mo9 O31 . . 2.200(3) yes Mo9 O32 . 2_656 1.953(4) yes Mo10 O30 . . 1.865(3) yes Mo10 O31 . . 2.150(3) yes Mo10 O33 . . 1.686(4) yes Mo10 O34 . . 1.760(4) yes Mo10 O35 . . 1.939(4) yes Mo10 O35 . 2_656 2.427(3) yes Mo11 O30 . 2_656 2.300(3) yes Mo11 O32 . . 1.926(4) yes Mo11 O35 . . 2.210(3) yes Mo11 O36 . . 1.706(5) yes Mo11 O37 . . 1.695(4) yes Mo11 O38 . . 1.964(3) yes Mo12 O25 . . 1.760(4) yes Mo12 O31 . . 1.880(4) yes Mo12 O34 . 2_656 2.218(4) yes Mo12 O35 . . 2.225(3) yes Mo12 O38 . . 1.896(4) yes Mo12 O39 . . 1.697(4) yes C2 O20 . 2_655 2.953(9) yes data_II _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H37.32 Mo8 N4 O30.66' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_iupac ? _chemical_formula_weight 1495.8 _chemical_melting_point ? _space_group_crystal_system triclinic _space_group_ssg_name 'P-1(\a\b\g)0' loop_ _space_group_symop_ssg_id _space_group_symop_ssg_operation_algebraic 1 x1,x2,x3,x4 2 -x1,-x2,-x3,-x4 _cell_length_a 7.8907(5) _cell_length_b 10.0855(3) _cell_length_c 12.4131(8) _cell_angle_alpha 113.685(4) _cell_angle_beta 92.857(7) _cell_angle_gamma 101.244(5) _cell_volume 878.20(9) _cell_formula_units_Z 1 _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _cell_measurement_temperature ? _cell_modulation_dimension 1 loop_ _cell_wave_vector_seq_id _cell_wave_vector_x _cell_wave_vector_y _cell_wave_vector_z 1 0.0633(3) -0.4284(5) -0.4159(6) _exptl_crystal_type_of_structure mod _exptl_crystal_description 'elongated block' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 2.8275 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_F_000 709 _exptl_absorpt_coefficient_mu 2.874 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details '(Jana2000; Petricek, Dusek & Palatinus, 2000)' _exptl_absorpt_correction_T_min 0.649 _exptl_absorpt_correction_T_max 0.826 _exptl_special_details ? _diffrn_ambient_temperature 293 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_source ? _diffrn_radiation_monochromator ? _diffrn_measurement_device_type 'Nonius CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 153057 _diffrn_reflns_av_R_equivalents 0.0643 _diffrn_reflns_av_unetI/netI 0.0388 _diffrn_reflns_theta_min 5.01 _diffrn_reflns_theta_max 35.93 _diffrn_reflns_theta_full 35.93 _diffrn_measured_fraction_theta_max ? _diffrn_measured_fraction_theta_full 0.96 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_reduction_process ? _diffrn_reflns_limit_index_m_1_max 2 _diffrn_reflns_limit_index_m_1_min -2 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _reflns_number_total 39145 _reflns_number_gt 21512 _reflns_threshold_expression 'I>2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_all 0.1076 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_gt 0.1194 _refine_ls_wR_factor_ref 0.1327 _refine_ls_goodness_of_fit_ref 1.34 _refine_ls_restrained_S_all ? _refine_ls_number_reflns 39145 _refine_ls_number_parameters 566 _refine_ls_number_restraints ? _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/(\s^2^(I)+0.001936I^2^)' _refine_ls_shift/su_max 0.0016 _refine_ls_shift/su_mean 0.0002 _refine_diff_density_max 2.11 _refine_diff_density_min -1.88 _refine_ls_extinction_method 'none' _refine_ls_extinction_coef ? loop_ _reflns_class_code _reflns_class_description _reflns_class_number_gt _reflns_class_R_factor_gt Main 'Main reflections' 6655 0.0344 Sat1 '1st-order satellites' 10636 0.0566 Sat2 '2nd-order satellites' 4221 0.1416 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Mo -1.683 0.686 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' O 0.011 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' C 0.003 0.002 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' N 0.006 0.003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' H 0.000 0.000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.1' _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement '(Jana2000; Petricek and Dusek, 2000)' _computing_molecular_graphics ? _computing_publication_material '(Jana2000; Petricek and Dusek, 2000)' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Mo Mo1 0.01475(2) 0.10641(2) 0.793165(14) 0.01834(6) Uani d . 1 . . Mo Mo2 0.41800(2) 0.149828(18) 0.739826(14) 0.01804(5) Uani d . 1 . . Mo Mo3 0.304037(18) 0.117739(17) 0.419560(14) 0.01527(5) Uani d . 1 . . Mo Mo4 -0.114145(19) 0.118717(16) 0.480196(13) 0.01409(5) Uani d . 1 . . O O1 -0.06329(17) 0.05779(15) 0.60558(12) 0.0165(4) Uani d . 1 . . O O2 -0.1051(2) 0.2348(2) 0.84722(16) 0.0333(6) Uani d . 1 . . O O3 -0.17194(18) -0.08043(17) 0.72417(13) 0.0206(5) Uani d . 1 . . O O4 0.0839(2) 0.0760(2) 0.91185(15) 0.0317(6) Uani d . 1 . . O O5 0.18520(18) -0.04563(16) 0.68331(12) 0.0185(4) Uani d . 1 . . O O6 0.22161(19) 0.23677(16) 0.78452(13) 0.0218(5) Uani d . 1 . . O O7 0.4736(2) 0.1296(2) 0.86514(15) 0.0343(7) Uani d . 1 . . O O8 0.55103(18) -0.00333(17) 0.64663(13) 0.0233(5) Uani d . 1 . . O O9 0.5569(2) 0.30712(19) 0.75102(17) 0.0328(6) Uani d . 1 . . O O10 0.30421(17) 0.08414(15) 0.55868(12) 0.0179(4) Uani d . 1 . . O O11 0.4254(2) 0.29384(18) 0.46168(15) 0.0260(5) Uani d . 1 . . O O12 0.09476(18) 0.23147(16) 0.49390(13) 0.0205(5) Uani d . 1 . . O O13 -0.2353(2) 0.24376(18) 0.54182(15) 0.0258(5) Uani d . 1 . . O O1w 0.2991(6) 0.4617(3) 0.3448(4) 0.0890(17) Uani d . 0.932(3) . . O O2w 0.3184(6) 0.1670(7) 0.1090(4) 0.0745(18) Uani d . 0.855(4) . . O O3w 0.2867(14) 0.4379(9) 0.0478(7) 0.129(5) Uani d . 0.554(16) . . N N1a 0.0186(3) 0.6031(3) 0.7674(3) 0.0327(8) Uani d . 0.487 . . N N2a 0.3348(6) 0.7035(6) 0.8312(5) 0.049(5) Uani d . 0.487 . . C C1a 0.0534(7) 0.7570(6) 0.8508(5) 0.0447(17) Uani d . 0.487 . . C C2a 0.1028(7) 0.5898(6) 0.6645(5) 0.049(2) Uani d . 0.487 . . C C3a 0.0843(7) 0.5154(7) 0.8242(6) 0.0554(19) Uani d . 0.487 . . C C4a 0.2446(7) 0.8174(6) 0.8873(5) 0.049(4) Uani d . 0.487 . . C C5a 0.2949(8) 0.6500(8) 0.7027(6) 0.067(5) Uani d . 0.487 . . C C6a 0.2787(7) 0.5790(7) 0.8664(6) 0.062(5) Uani d . 0.487 . . H H1a -0.1000(3) 0.5690(3) 0.7435(3) 0.0481(15) Uani d . 0.487 . . H H2a 0.4527(3) 0.7440(3) 0.8547(3) 0.076(9) Uani d . 0.487 . . H H3a -0.0027(3) 0.7650(3) 0.9203(3) 0.074(3) Uani d . 0.487 . . H H4a 0.0075(3) 0.8137(3) 0.8140(3) 0.065(3) Uani d . 0.487 . . H H5a 0.0585(3) 0.6464(3) 0.6269(3) 0.066(3) Uani d . 0.487 . . H H6a 0.0798(3) 0.4857(3) 0.6091(3) 0.075(3) Uani d . 0.487 . . H H7a 0.0642(3) 0.4124(3) 0.7669(3) 0.082(3) Uani d . 0.487 . . H H8a 0.0241(3) 0.5213(3) 0.8916(3) 0.083(3) Uani d . 0.487 . . H H9a 0.2824(3) 0.8988(3) 0.8646(3) 0.073(5) Uani d . 0.487 . . H H10a 0.2714(3) 0.8547(3) 0.9729(3) 0.072(5) Uani d . 0.487 . . H H11a 0.3551(3) 0.5721(3) 0.6636(3) 0.106(8) Uani d . 0.487 . . H H12a 0.3342(3) 0.7315(3) 0.6804(3) 0.095(7) Uani d . 0.487 . . H H13a 0.3006(3) 0.6165(3) 0.9522(3) 0.084(6) Uani d . 0.487 . . H H14a 0.3412(3) 0.5023(3) 0.8286(3) 0.098(7) Uani d . 0.487 . . N N1b 0.2228(8) 0.5251(4) 0.8063(4) 0.087(3) Uani d . 0.513 . . N N2b 0.2257(11) 0.7672(6) 0.8018(6) 0.068(18) Uani d . 0.513 . . C C1b 0.2981(11) 0.5322(7) 0.7048(6) 0.149(8) Uani d . 0.513 . . C C2b 0.3241(11) 0.6415(7) 0.9140(6) 0.256(10) Uani d . 0.513 . . C C3b 0.0412(12) 0.5424(7) 0.7988(7) 0.306(11) Uani d . 0.513 . . C C4b 0.3020(11) 0.6795(7) 0.7040(6) 0.158(17) Uani d . 0.513 . . C C5b 0.3256(13) 0.7887(7) 0.9120(7) 0.29(2) Uani d . 0.513 . . C C6b 0.0414(13) 0.6900(7) 0.7931(7) 0.22(2) Uani d . 0.513 . . H H1b 0.2259(8) 0.4347(4) 0.8070(4) 0.128(5) Uani d . 0.513 . . H H2b 0.2307(8) 0.8579(4) 0.7995(4) 0.10(3) Uani d . 0.513 . . H H3b 0.2284(8) 0.4541(4) 0.6326(4) 0.341(13) Uani d . 0.513 . . H H4b 0.4160(8) 0.5183(4) 0.7090(4) 0.272(16) Uani d . 0.513 . . H H5b 0.4428(8) 0.6293(4) 0.9192(4) 0.375(18) Uani d . 0.513 . . H H6b 0.2720(8) 0.6368(4) 0.9819(4) 0.505(13) Uani d . 0.513 . . H H7b -0.0077(8) 0.5410(4) 0.8686(4) 0.567(17) Uani d . 0.513 . . H H8b -0.0280(8) 0.4616(4) 0.7277(4) 0.51(2) Uani d . 0.513 . . H H9b 0.4219(8) 0.7308(4) 0.7097(4) 0.35(3) Uani d . 0.513 . . H H10b 0.2373(8) 0.6655(4) 0.6302(4) 0.31(2) Uani d . 0.513 . . H H11b 0.2745(8) 0.8479(4) 0.9791(4) 0.54(3) Uani d . 0.513 . . H H12b 0.4450(8) 0.8411(4) 0.9177(4) 0.50(4) Uani d . 0.513 . . H H13b -0.0227(8) 0.6719(4) 0.7179(4) 0.34(3) Uani d . 0.513 . . H H14b -0.0101(8) 0.7505(4) 0.8594(4) 0.42(3) Uani d . 0.513 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 _atom_site_aniso_type_symbol Mo1 0.01765(7) 0.02411(8) 0.01514(7) 0.00836(6) 0.00484(5) 0.00828(6) Mo Mo2 0.01580(7) 0.02150(7) 0.01672(7) 0.00599(5) 0.00213(5) 0.00724(6) Mo Mo3 0.01236(6) 0.01932(7) 0.01823(7) 0.00569(5) 0.00447(5) 0.01086(6) Mo Mo4 0.01378(6) 0.01632(6) 0.01532(7) 0.00663(5) 0.00372(5) 0.00822(5) Mo O1 0.0160(5) 0.0198(5) 0.0162(5) 0.0059(4) 0.0029(4) 0.0093(4) O O2 0.0317(8) 0.0347(8) 0.0328(9) 0.0180(7) 0.0112(7) 0.0079(7) O O3 0.0180(6) 0.0297(7) 0.0203(6) 0.0068(5) 0.0041(5) 0.0159(5) O O4 0.0331(8) 0.0440(9) 0.0226(7) 0.0111(7) 0.0048(6) 0.0176(7) O O5 0.0185(6) 0.0244(6) 0.0176(6) 0.0089(5) 0.0042(5) 0.0118(5) O O6 0.0194(6) 0.0212(6) 0.0235(7) 0.0084(5) 0.0053(5) 0.0063(5) O O7 0.0341(9) 0.0518(10) 0.0235(8) 0.0176(8) 0.0022(6) 0.0191(7) O O8 0.0188(6) 0.0308(7) 0.0251(7) 0.0140(5) 0.0075(5) 0.0124(6) O O9 0.0246(7) 0.0270(7) 0.0414(9) 0.0020(6) 0.0044(7) 0.0108(7) O O10 0.0156(5) 0.0216(6) 0.0181(6) 0.0044(4) 0.0023(4) 0.0100(5) O O11 0.0210(6) 0.0239(6) 0.0352(8) 0.0028(5) 0.0051(6) 0.0155(6) O O12 0.0172(6) 0.0201(6) 0.0266(7) 0.0062(5) 0.0058(5) 0.0110(5) O O13 0.0269(7) 0.0267(7) 0.0282(7) 0.0167(6) 0.0080(6) 0.0108(6) O O1w 0.096(3) 0.0367(13) 0.114(3) 0.0113(15) -0.036(2) 0.0194(16) O O2w 0.0485(17) 0.120(3) 0.0554(18) -0.0029(19) -0.0035(14) 0.048(2) O O3w 0.169(10) 0.092(6) 0.077(5) -0.019(5) -0.014(5) 0.013(4) O N1a 0.0295(9) 0.0334(10) 0.0397(12) 0.0061(8) 0.0042(8) 0.0205(9) N N2a 0.0284(11) 0.060(8) 0.065(9) 0.006(2) 0.005(2) 0.037(7) N C1a 0.043(4) 0.0424(12) 0.044(2) 0.019(2) 0.002(2) 0.0094(13) C C2a 0.057(3) 0.053(4) 0.032(2) 0.009(3) 0.009(2) 0.016(2) C C3a 0.051(2) 0.052(3) 0.081(3) 0.001(2) -0.0018(18) 0.052(2) C C4a 0.050(5) 0.039(4) 0.050(6) 0.001(4) -0.012(4) 0.017(4) C C5a 0.0504(19) 0.094(8) 0.060(8) 0.013(3) 0.030(3) 0.036(7) C C6a 0.049(2) 0.064(8) 0.093(6) 0.015(3) -0.008(3) 0.054(6) C H1a 0.0309(9) 0.050(2) 0.063(2) 0.0024(10) -0.0015(10) 0.0273(18) H H2a 0.0292(13) 0.096(13) 0.107(15) 0.000(3) 0.000(4) 0.056(12) H H3a 0.060(7) 0.095(3) 0.051(2) 0.034(4) 0.020(3) 0.0075(19) H H4a 0.065(5) 0.0394(16) 0.081(4) 0.026(2) -0.016(3) 0.0125(19) H H5a 0.083(4) 0.078(5) 0.040(3) 0.000(4) -0.007(3) 0.036(3) H H6a 0.088(6) 0.066(4) 0.046(2) 0.021(5) 0.009(3) -0.003(2) H H7a 0.080(4) 0.042(2) 0.132(5) 0.002(3) -0.017(3) 0.053(3) H H8a 0.070(4) 0.111(4) 0.098(3) -0.012(4) 0.004(3) 0.089(3) H H9a 0.075(6) 0.040(4) 0.093(10) -0.014(4) -0.030(6) 0.033(5) H H10a 0.076(9) 0.065(5) 0.049(6) 0.005(6) -0.021(6) 0.007(4) H H11a 0.071(4) 0.143(12) 0.095(11) 0.043(7) 0.053(6) 0.029(10) H H12a 0.074(3) 0.142(11) 0.082(12) -0.009(5) 0.031(5) 0.074(10) H H13a 0.074(4) 0.103(11) 0.099(7) 0.006(6) -0.025(4) 0.079(7) H H14a 0.070(3) 0.078(11) 0.161(11) 0.038(5) -0.013(4) 0.060(9) H N1b 0.141(6) 0.0365(17) 0.112(3) 0.043(3) 0.061(3) 0.044(2) N N2b 0.11(4) 0.038(6) 0.067(19) 0.027(14) 0.01(2) 0.034(9) N C1b 0.303(14) 0.140(10) 0.099(10) 0.175(9) 0.117(10) 0.080(9) C C2b 0.61(2) 0.081(7) 0.074(8) 0.128(11) -0.082(10) 0.024(6) C C3b 0.15(3) 0.180(8) 0.762(12) 0.093(12) 0.207(13) 0.331(8) C C4b 0.25(3) 0.204(16) 0.19(2) 0.194(18) 0.17(2) 0.177(16) C C5b 0.62(5) 0.041(9) 0.14(2) 0.070(18) -0.20(2) -0.008(12) C C6b 0.13(5) 0.154(8) 0.523(18) 0.097(17) 0.17(2) 0.241(10) C H1b 0.177(12) 0.052(2) 0.207(5) 0.060(4) 0.094(6) 0.083(3) H H2b 0.13(7) 0.059(10) 0.14(3) 0.03(2) 0.01(4) 0.072(16) H H3b 0.79(2) 0.180(17) 0.066(10) 0.310(16) 0.005(11) -0.016(11) H H4b 0.36(3) 0.314(17) 0.46(2) 0.306(16) 0.34(2) 0.346(17) H H5b 0.56(4) 0.108(13) 0.381(16) 0.01(2) -0.349(18) 0.104(12) H H6b 1.35(3) 0.260(16) 0.083(9) 0.481(18) 0.181(12) 0.115(10) H H7b 0.51(3) 0.462(16) 1.30(2) 0.415(18) 0.73(2) 0.741(17) H H8b 0.14(5) 0.178(13) 1.241(19) -0.06(2) -0.13(2) 0.378(13) H H9b 0.28(5) 0.42(3) 0.79(4) 0.31(3) 0.40(4) 0.56(3) H H10b 0.70(5) 0.32(3) 0.10(2) 0.40(3) 0.19(2) 0.15(2) H H11b 1.40(7) 0.143(16) 0.07(3) 0.37(3) -0.08(3) -0.027(18) H H12b 0.58(8) 0.073(16) 0.67(4) -0.09(3) -0.54(4) 0.13(2) H H13b 0.10(7) 0.174(15) 0.77(2) 0.00(3) -0.11(3) 0.253(14) H H14b 0.48(7) 0.363(15) 0.88(3) 0.38(3) 0.59(3) 0.522(18) H loop_ _atom_site_Fourier_wave_vector_seq_id _atom_site_Fourier_wave_vector_x _atom_site_Fourier_wave_vector_y _atom_site_Fourier_wave_vector_z 1 0.06330 -0.4284 -0.41590 2 0.12660 -0.8568 -0.83180 3 0.18990 -1.2852 -1.24770 loop_ _atom_site_occ_Fourier_id _atom_site_occ_Fourier_atom_site_label _atom_site_occ_Fourier_wave_vector_seq_id O3wo1 O3w 1 loop_ _atom_site_occ_Fourier_param_id _atom_site_occ_Fourier_param_cos _atom_site_occ_Fourier_param_sin O3wo1 0.008(10) -0.013(10) loop_ _atom_site_displace_Fourier_id _atom_site_displace_Fourier_atom_site_label _atom_site_displace_Fourier_axis _atom_site_displace_Fourier_wave_vector_seq_id Mo1x1 Mo1 x 1 Mo1y1 Mo1 y 1 Mo1z1 Mo1 z 1 Mo1x2 Mo1 x 2 Mo1y2 Mo1 y 2 Mo1z2 Mo1 z 2 Mo1x3 Mo1 x 3 Mo1y3 Mo1 y 3 Mo1z3 Mo1 z 3 Mo2x1 Mo2 x 1 Mo2y1 Mo2 y 1 Mo2z1 Mo2 z 1 Mo2x2 Mo2 x 2 Mo2y2 Mo2 y 2 Mo2z2 Mo2 z 2 Mo2x3 Mo2 x 3 Mo2y3 Mo2 y 3 Mo2z3 Mo2 z 3 Mo3x1 Mo3 x 1 Mo3y1 Mo3 y 1 Mo3z1 Mo3 z 1 Mo3x2 Mo3 x 2 Mo3y2 Mo3 y 2 Mo3z2 Mo3 z 2 Mo3x3 Mo3 x 3 Mo3y3 Mo3 y 3 Mo3z3 Mo3 z 3 Mo4x1 Mo4 x 1 Mo4y1 Mo4 y 1 Mo4z1 Mo4 z 1 Mo4x2 Mo4 x 2 Mo4y2 Mo4 y 2 Mo4z2 Mo4 z 2 Mo4x3 Mo4 x 3 Mo4y3 Mo4 y 3 Mo4z3 Mo4 z 3 O1x1 O1 x 1 O1y1 O1 y 1 O1z1 O1 z 1 O1x2 O1 x 2 O1y2 O1 y 2 O1z2 O1 z 2 O2x1 O2 x 1 O2y1 O2 y 1 O2z1 O2 z 1 O2x2 O2 x 2 O2y2 O2 y 2 O2z2 O2 z 2 O3x1 O3 x 1 O3y1 O3 y 1 O3z1 O3 z 1 O3x2 O3 x 2 O3y2 O3 y 2 O3z2 O3 z 2 O4x1 O4 x 1 O4y1 O4 y 1 O4z1 O4 z 1 O4x2 O4 x 2 O4y2 O4 y 2 O4z2 O4 z 2 O5x1 O5 x 1 O5y1 O5 y 1 O5z1 O5 z 1 O5x2 O5 x 2 O5y2 O5 y 2 O5z2 O5 z 2 O6x1 O6 x 1 O6y1 O6 y 1 O6z1 O6 z 1 O6x2 O6 x 2 O6y2 O6 y 2 O6z2 O6 z 2 O7x1 O7 x 1 O7y1 O7 y 1 O7z1 O7 z 1 O7x2 O7 x 2 O7y2 O7 y 2 O7z2 O7 z 2 O8x1 O8 x 1 O8y1 O8 y 1 O8z1 O8 z 1 O8x2 O8 x 2 O8y2 O8 y 2 O8z2 O8 z 2 O9x1 O9 x 1 O9y1 O9 y 1 O9z1 O9 z 1 O9x2 O9 x 2 O9y2 O9 y 2 O9z2 O9 z 2 O10x1 O10 x 1 O10y1 O10 y 1 O10z1 O10 z 1 O10x2 O10 x 2 O10y2 O10 y 2 O10z2 O10 z 2 O11x1 O11 x 1 O11y1 O11 y 1 O11z1 O11 z 1 O11x2 O11 x 2 O11y2 O11 y 2 O11z2 O11 z 2 O12x1 O12 x 1 O12y1 O12 y 1 O12z1 O12 z 1 O12x2 O12 x 2 O12y2 O12 y 2 O12z2 O12 z 2 O13x1 O13 x 1 O13y1 O13 y 1 O13z1 O13 z 1 O13x2 O13 x 2 O13y2 O13 y 2 O13z2 O13 z 2 O1wx1 O1w x 1 O1wy1 O1w y 1 O1wz1 O1w z 1 O1wx2 O1w x 2 O1wy2 O1w y 2 O1wz2 O1w z 2 O2wx1 O2w x 1 O2wy1 O2w y 1 O2wz1 O2w z 1 O2wx2 O2w x 2 O2wy2 O2w y 2 O2wz2 O2w z 2 O3wx1 O3w x 1 O3wy1 O3w y 1 O3wz1 O3w z 1 loop_ _atom_site_displace_Fourier_param_id _atom_site_displace_Fourier_param_cos _atom_site_displace_Fourier_param_sin Mo1x1 0.01299(3) 0.00173(3) Mo1y1 0.02001(3) -0.01539(3) Mo1z1 0.01094(2) 0.00305(2) Mo1x2 0.00081(5) -0.00261(5) Mo1y2 -0.00031(4) -0.00121(4) Mo1z2 -0.00233(3) 0.00154(3) Mo1x3 0.00152(11) 0.00161(11) Mo1y3 0.00709(7) 0.00131(7) Mo1z3 -0.00063(6) 0.00391(6) Mo2x1 0.01297(3) 0.00311(3) Mo2y1 0.01608(3) -0.00520(2) Mo2z1 0.00942(2) 0.006949(19) Mo2x2 0.00137(5) -0.00158(5) Mo2y2 0.00030(4) -0.00037(4) Mo2z2 -0.00234(3) 0.00187(3) Mo2x3 0.00190(13) 0.00096(13) Mo2y3 0.00324(9) 0.00126(9) Mo2z3 -0.00103(7) 0.00215(7) Mo3x1 -0.00328(3) 0.01086(3) Mo3y1 -0.00814(2) 0.01121(2) Mo3z1 -0.006788(18) 0.01144(2) Mo3x2 -0.00048(4) 0.00181(4) Mo3y2 -0.00053(4) 0.00052(4) Mo3z2 -0.00077(3) -0.00295(3) Mo3x3 -0.00084(14) 0.00116(14) Mo3y3 0.00135(10) -0.00132(11) Mo3z3 0.00063(8) -0.00338(8) Mo4x1 0.00040(3) 0.01207(3) Mo4y1 -0.00370(2) 0.01270(2) Mo4z1 -0.004949(18) 0.013123(19) Mo4x2 0.00112(4) 0.00152(4) Mo4y2 0.00023(3) 0.00067(3) Mo4z2 -0.00144(3) -0.00231(3) Mo4x3 -0.00086(13) 0.00173(13) Mo4y3 -0.00032(10) -0.00088(10) Mo4z3 -0.00157(7) -0.00306(7) O1x1 0.0056(2) 0.0095(2) O1y1 0.01093(19) 0.00797(19) O1z1 0.00426(15) 0.01190(16) O1x2 0.0013(3) 0.0008(3) O1y2 0.0007(3) 0.0005(3) O1z2 -0.0022(2) -0.0020(2) O2x1 0.0127(3) -0.0048(3) O2y1 0.0096(3) -0.0262(3) O2z1 0.0142(2) 0.0086(2) O2x2 -0.0032(5) -0.0010(5) O2y2 -0.0024(4) 0.0007(4) O2z2 0.0009(3) 0.0029(3) O3x1 0.0098(2) 0.0078(2) O3y1 0.0243(2) -0.0001(2) O3z1 0.01429(17) 0.00542(17) O3x2 0.0029(4) -0.0006(4) O3y2 0.0019(3) -0.0022(3) O3z2 -0.0021(2) -0.0030(2) O4x1 0.0123(3) 0.0044(3) O4y1 0.0182(3) -0.0345(3) O4z1 0.0129(2) -0.0073(2) O4x2 -0.0002(5) -0.0043(4) O4y2 -0.0040(4) -0.0022(4) O4z2 -0.0027(3) 0.0023(3) O5x1 0.0080(2) 0.0105(2) O5y1 0.0223(2) 0.0033(2) O5z1 0.01257(16) 0.00746(16) O5x2 0.0014(4) 0.0004(4) O5y2 0.0009(3) -0.0005(3) O5z2 -0.0016(2) -0.0026(2) O6x1 0.0133(3) -0.0018(3) O6y1 0.0148(2) -0.0153(2) O6z1 0.01106(18) 0.00607(18) O6x2 -0.0014(4) -0.0026(4) O6y2 -0.0003(3) -0.0013(3) O6z2 -0.0012(2) 0.0036(2) O7x1 0.0153(3) -0.0039(3) O7y1 0.0219(3) -0.0217(3) O7z1 0.0136(2) -0.0003(2) O7x2 -0.0011(5) -0.0014(5) O7y2 0.0004(4) 0.0022(4) O7z2 -0.0017(3) 0.0046(3) O8x1 0.0054(2) 0.0098(2) O8y1 0.0122(2) 0.0066(2) O8z1 0.00748(18) 0.00990(18) O8x2 0.0013(4) 0.0003(4) O8y2 0.0000(3) -0.0004(3) O8z2 -0.0027(3) -0.0018(3) O9x1 0.0128(3) 0.0003(3) O9y1 0.0118(2) -0.0082(2) O9z1 0.0085(2) 0.0109(2) O9x2 -0.0001(4) -0.0024(4) O9y2 0.0007(4) -0.0004(4) O9z2 -0.0005(3) 0.0029(3) O10x1 0.0039(2) 0.0107(2) O10y1 0.00840(19) 0.00922(19) O10z1 0.00156(16) 0.01162(16) O10x2 0.0011(3) 0.0019(3) O10y2 0.0004(3) 0.0004(3) O10z2 -0.0020(2) -0.0019(2) O11x1 -0.0016(3) 0.0136(3) O11y1 -0.0017(2) 0.0141(2) O11z1 -0.0073(2) 0.0172(2) O11x2 0.0014(4) 0.0016(4) O11y2 0.0006(3) 0.0015(3) O11z2 -0.0039(3) -0.0005(3) O12x1 0.0013(2) 0.0125(2) O12y1 0.0006(2) 0.0138(2) O12z1 -0.00535(18) 0.01749(18) O12x2 0.0018(4) 0.0003(4) O12y2 -0.0007(3) 0.0001(3) O12z2 -0.0038(2) -0.0008(2) O13x1 0.0031(3) 0.0139(3) O13y1 0.0023(2) 0.0145(2) O13z1 -0.00192(19) 0.01862(19) O13x2 0.0012(4) 0.0002(4) O13y2 -0.0003(3) -0.0002(3) O13z2 -0.0028(3) 0.0002(3) O1wx1 0.0149(7) -0.0173(7) O1wy1 -0.0075(4) -0.0003(4) O1wz1 -0.0189(5) 0.0183(5) O1wx2 0.0036(9) 0.0028(11) O1wy2 0.0007(6) -0.0026(7) O1wz2 -0.0033(6) -0.0021(7) O2wx1 0.0341(10) 0.0095(7) O2wy1 -0.0488(12) -0.0338(8) O2wz1 -0.0052(6) -0.0105(4) O2wx2 -0.0147(9) -0.0035(9) O2wy2 0.0144(10) 0.0137(11) O2wz2 0.0024(6) 0.0011(6) O3wx1 -0.0057(16) -0.0071(15) O3wy1 -0.0208(11) -0.0143(11) O3wz1 0.0102(8) -0.0075(8) loop_ _atom_site_U_Fourier_id _atom_site_U_Fourier_atom_site_label _atom_site_U_Fourier_tens_elem _atom_site_U_Fourier_wave_vector_seq_id Mo1U111 Mo1 U11 1 Mo1U221 Mo1 U22 1 Mo1U331 Mo1 U33 1 Mo1U121 Mo1 U12 1 Mo1U131 Mo1 U13 1 Mo1U231 Mo1 U23 1 Mo2U111 Mo2 U11 1 Mo2U221 Mo2 U22 1 Mo2U331 Mo2 U33 1 Mo2U121 Mo2 U12 1 Mo2U131 Mo2 U13 1 Mo2U231 Mo2 U23 1 Mo3U111 Mo3 U11 1 Mo3U221 Mo3 U22 1 Mo3U331 Mo3 U33 1 Mo3U121 Mo3 U12 1 Mo3U131 Mo3 U13 1 Mo3U231 Mo3 U23 1 Mo4U111 Mo4 U11 1 Mo4U221 Mo4 U22 1 Mo4U331 Mo4 U33 1 Mo4U121 Mo4 U12 1 Mo4U131 Mo4 U13 1 Mo4U231 Mo4 U23 1 loop_ _atom_site_U_Fourier_param_id _atom_site_U_Fourier_param_cos _atom_site_U_Fourier_param_sin Mo1U111 -0.00125(10) -0.00118(10) Mo1U221 -0.00077(13) 0.00009(11) Mo1U331 -0.00198(10) -0.00038(10) Mo1U121 -0.00084(9) 0.00031(8) Mo1U131 -0.00076(8) -0.00047(8) Mo1U231 -0.00225(9) 0.00037(8) Mo2U111 -0.00106(10) -0.00049(9) Mo2U221 -0.00170(10) 0.00150(9) Mo2U331 -0.00069(10) 0.00119(10) Mo2U121 -0.00090(8) 0.00006(7) Mo2U131 -0.00063(8) 0.00129(8) Mo2U231 -0.00173(8) 0.00111(8) Mo3U111 -0.00038(9) 0.00037(8) Mo3U221 -0.00037(8) 0.00086(9) Mo3U331 -0.00180(10) 0.00241(11) Mo3U121 -0.00008(7) 0.00035(7) Mo3U131 -0.00041(7) 0.00100(8) Mo3U231 -0.00080(7) 0.00177(8) Mo4U111 -0.00099(9) 0.00016(8) Mo4U221 -0.00073(8) 0.00047(8) Mo4U331 -0.00033(9) 0.00225(10) Mo4U121 -0.00088(7) 0.00027(7) Mo4U131 -0.00061(7) 0.00057(7) Mo4U231 -0.00046(7) 0.00109(7) loop_ _atom_site_occ_special_func_atom_site_label _atom_site_occ_special_func_crenel_c _atom_site_occ_special_func_crenel_w O1w 0.866(6) 0.932(3) O2w 0.067(4) 0.855(4) N1a 0.0835 0.487 N2a 0.0835 0.487 C1a 0.0835 0.487 C2a 0.0835 0.487 C3a 0.0835 0.487 C4a 0.0835 0.487 C5a 0.0835 0.487 C6a 0.0835 0.487 H1a 0.0835 0.487 H2a 0.0835 0.487 H3a 0.0835 0.487 H4a 0.0835 0.487 H5a 0.0835 0.487 H6a 0.0835 0.487 H7a 0.0835 0.487 H8a 0.0835 0.487 H9a 0.0835 0.487 H10a 0.0835 0.487 H11a 0.0835 0.487 H12a 0.0835 0.487 H13a 0.0835 0.487 H14a 0.0835 0.487 N1b 0.6136 0.513 N2b 0.6136 0.513 C1b 0.6136 0.513 C2b 0.6136 0.513 C3b 0.6136 0.513 C4b 0.6136 0.513 C5b 0.6136 0.513 C6b 0.6136 0.513 H1b 0.6136 0.513 H2b 0.6136 0.513 H3b 0.6136 0.513 H4b 0.6136 0.513 H5b 0.6136 0.513 H6b 0.6136 0.513 H7b 0.6136 0.513 H8b 0.6136 0.513 H9b 0.6136 0.513 H10b 0.6136 0.513 H11b 0.6136 0.513 H12b 0.6136 0.513 H13b 0.6136 0.513 H14b 0.6136 0.513 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag _geom_bond_distance_max _geom_bond_distance_min _geom_bond_distance_av O1w O9 . 2_666 yes 3.232(17) 2.924(16) 3.073(16) O1w O11 . . yes 2.960(17) 2.885(16) 2.918(17) O1w O11 . 2_666 yes 3.191(12) 2.888(12) 3.031(12) O1w O13 . 2_566 yes 2.951(13) 2.823(12) 2.905(12) O1w O2w . . yes 3.502(18) 3.068(19) 3.341(19) O1w O3w . . yes 4.15(2) 3.11(2) 3.56(2) O2w O3 . 2_556 yes 3.00(2) 2.662(18) 2.770(19) O2w O4 . 1_554 yes 2.867(15) 2.595(14) 2.753(16) O2w O7 . 1_554 yes 3.459(17) 3.046(19) 3.222(17) O2w O3w . . yes 3.49(3) 2.75(3) 3.26(3) O3w O6 . 1_554 yes 3.075(12) 2.970(12) 3.028(12) O3w O9 . 2_666 yes 2.840(12) 2.755(11) 2.787(12)