#------------------------------------------------------------------------------ #$Date: 2016-02-14 14:26:36 +0000 (Sun, 14 Feb 2016) $ #$Revision: 176435 $ #$URL: svn://www.crystallography.net/cod/cif/1/50/77/1507785.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1507785 loop_ _publ_author_name 'Salles, L' 'Piquemal, J Y' 'Mahha, Y' 'Gentil, M' 'Herson, P' 'Bregeault, M' _publ_section_title ; Crystal structures of three novel dioxotetraperoxodi(molybdenum) heteropolyanions in [PPh4]2[R2SiO2{Mo2O2(mu-O2)2(O2)2}] (R2 = (CH3)2, (i-C4H9)2 or (CH3)(CH2Cl)) and characterization of their tungsten analogues ; _journal_issue 17 _journal_name_full Polyhedron _journal_page_first 4786 _journal_page_last 4792 _journal_paper_doi 10.1016/j.poly.2007.06.007 _journal_volume 26 _journal_year 2007 _chemical_compound_source ; ? ; _chemical_formula_moiety ' (C2 H5 Cl1 Mo2 O12 Si)2-,2(C24 H20 P)+ ' _chemical_formula_sum 'C50 H45 Cl Mo2 O12 P2 Si' _chemical_formula_weight 1155.22 _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _cell_angle_alpha 76.03(2) _cell_angle_beta 79.39(2) _cell_angle_gamma 61.18(2) _cell_formula_units_Z 2 _cell_length_a 13.467(3) _cell_length_b 13.548(3) _cell_length_c 15.931(3) _cell_measurement_reflns_used 25 _cell_measurement_temperature 295 _cell_measurement_theta_max 15.4 _cell_measurement_theta_min 15 _cell_volume 2463.4(10) _computing_cell_refinement ; Cad4 Express, (Enraf-Nonius, 1989) ; _computing_data_collection ; Cad4 Express, (Enraf-Nonius, 1989) ; _computing_data_reduction ; RC93 (Watkin, Prout & Lilley, 1994) ; _computing_molecular_graphics ; CAMERON (Watkin et al 1996) ; _computing_publication_material ; CRYSTALS (Watkin et al 2001) ; _computing_structure_refinement ; CRYSTALS (Watkin et al 2001) ; _computing_structure_solution ; SHELXS 86 (Sheldrick, 1986) ; _diffrn_ambient_temperature 295 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type ; Enraf-Nonius CAD4 ; _diffrn_measurement_method \w/2\q _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 10103 _diffrn_reflns_theta_full 25.976 _diffrn_reflns_theta_max 25.976 _diffrn_reflns_theta_min 1.321 _diffrn_standards_decay_% 7.79 _diffrn_standards_interval_time 3600 _diffrn_standards_number 2 _exptl_absorpt_coefficient_mu 0.715 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_correction_T_min 0.63 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details ; Azimutal absorption correction (North et al, 1968) ; _exptl_crystal_colour ' yellow ' _exptl_crystal_density_diffrn 1.557 _exptl_crystal_description ' parallelepiped ' _exptl_crystal_F_000 1172.000 _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.11 _refine_diff_density_max 1.41 _refine_diff_density_min -1.49 _refine_ls_extinction_coef 723.5 _refine_ls_extinction_method 'Larson 1970 Crystallographic Computing eq 22' _refine_ls_goodness_of_fit_ref 1.0605 _refine_ls_hydrogen_treatment refU _refine_ls_matrix_type full _refine_ls_number_parameters 615 _refine_ls_number_reflns 7933 _refine_ls_R_factor_all 0.0637 _refine_ls_R_factor_gt 0.0533 _refine_ls_shift/su_max 0.001373 _refine_ls_structure_factor_coef F _refine_ls_weighting_details ; Method = Prince modified Chebychev polynomial, (Watkin, 1994) W = [weight] * [1-(deltaF/6*sigmaF)^2]^2 8.83 0.697 7.24 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.0589 _refine_ls_wR_factor_gt 0.0583 _refine_ls_wR_factor_ref 0.0583 _reflns_limit_h_max 16 _reflns_limit_h_min -16 _reflns_limit_k_max 16 _reflns_limit_k_min -15 _reflns_limit_l_max 19 _reflns_limit_l_min 0 _reflns_number_gt 7931 _reflns_number_total 9666 _reflns_threshold_expression I>3.00u(I) _cod_data_source_file LS_5cif.cif _cod_data_source_block LS-5 _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to the built-in table from CIF Core dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_formula_sum ' C50 H45 Cl1 Mo2 O12 P2 Si ' _cod_database_code 1507785 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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_occupancy _atom_site_adp_type Mo1 Mo 0.188755(19) 0.34425(2) 0.736801(16) 0.0357 1.0000 Uani Mo2 Mo 0.31301(2) 0.03559(2) 0.795225(17) 0.0398 1.0000 Uani Si1 Si 0.45995(6) 0.18146(7) 0.74509(6) 0.0394 1.0000 Uani P1 P 0.64489(6) -0.45885(7) 0.82408(5) 0.0365 1.0000 Uani P2 P -0.05004(6) 0.88836(6) 0.68158(5) 0.0340 1.0000 Uani Cl1 Cl 0.50084(9) 0.3500(1) 0.60180(7) 0.0730 1.0000 Uani O1 O 0.1828(2) 0.4480(2) 0.65159(18) 0.0605 1.0000 Uani O2 O 0.13933(19) 0.4202(2) 0.83539(17) 0.0524 1.0000 Uani O3 O 0.0463(2) 0.4157(2) 0.80369(19) 0.0597 1.0000 Uani O4 O 0.1222(2) 0.2760(2) 0.68843(17) 0.0538 1.0000 Uani O5 O 0.2461(2) 0.2084(2) 0.67981(14) 0.0463 1.0000 Uani O6 O 0.34317(16) 0.29095(18) 0.76760(14) 0.0413 1.0000 Uani O7 O 0.44349(18) 0.06766(19) 0.76347(17) 0.0484 1.0000 Uani O8 O 0.22809(17) 0.17629(19) 0.84966(14) 0.0416 1.0000 Uani O9 O 0.1596(2) 0.1202(2) 0.84355(17) 0.0522 1.0000 Uani O10 O 0.2502(3) -0.0219(3) 0.7321(2) 0.0703 1.0000 Uani O11 O 0.3659(3) -0.0408(3) 0.6966(2) 0.0694 1.0000 Uani O12 O 0.3642(2) -0.0693(2) 0.88069(19) 0.0644 1.0000 Uani C1 C 0.4999(3) 0.2130(3) 0.6262(3) 0.0579 1.0000 Uani C2 C 0.5740(3) 0.1592(4) 0.8085(3) 0.0613 1.0000 Uani C11 C 0.7181(3) -0.6050(3) 0.8778(2) 0.0405 1.0000 Uani C12 C 0.8360(3) -0.6568(3) 0.8805(3) 0.0565 1.0000 Uani C13 C 0.8926(3) -0.7687(4) 0.9235(3) 0.0671 1.0000 Uani C14 C 0.8332(4) -0.8301(3) 0.9617(3) 0.0672 1.0000 Uani C15 C 0.7179(4) -0.7797(4) 0.9597(3) 0.0658 1.0000 Uani C16 C 0.6598(3) -0.6672(3) 0.9194(2) 0.0535 1.0000 Uani C21 C 0.7119(3) -0.4377(3) 0.71752(19) 0.0397 1.0000 Uani C22 C 0.8170(3) -0.4369(3) 0.7084(2) 0.0495 1.0000 Uani C23 C 0.8718(3) -0.4261(4) 0.6272(3) 0.0595 1.0000 Uani C24 C 0.8227(4) -0.4137(4) 0.5544(2) 0.0628 1.0000 Uani C25 C 0.7193(4) -0.4132(4) 0.5622(2) 0.0636 1.0000 Uani C26 C 0.6634(3) -0.4259(3) 0.6437(2) 0.0528 1.0000 Uani C31 C 0.6483(2) -0.3672(3) 0.88631(19) 0.0392 1.0000 Uani C32 C 0.6253(3) -0.2553(3) 0.8473(2) 0.0478 1.0000 Uani C33 C 0.6202(3) -0.1814(3) 0.8966(3) 0.0554 1.0000 Uani C34 C 0.6392(3) -0.2186(4) 0.9830(3) 0.0580 1.0000 Uani C35 C 0.6641(4) -0.3301(4) 1.0211(2) 0.0621 1.0000 Uani C36 C 0.6673(3) -0.4043(3) 0.9737(2) 0.0523 1.0000 Uani C41 C 0.5003(2) -0.4259(3) 0.8164(2) 0.0400 1.0000 Uani C42 C 0.4115(3) -0.3282(3) 0.8446(2) 0.0503 1.0000 Uani C43 C 0.3001(3) -0.3092(4) 0.8431(3) 0.0597 1.0000 Uani C44 C 0.2791(3) -0.3851(4) 0.8148(2) 0.0573 1.0000 Uani C45 C 0.3676(3) -0.4796(3) 0.7845(2) 0.0528 1.0000 Uani C46 C 0.4777(3) -0.5000(3) 0.7849(2) 0.0469 1.0000 Uani C51 C -0.1448(3) 0.8829(3) 0.61885(19) 0.0380 1.0000 Uani C52 C -0.1154(3) 0.8743(3) 0.5313(2) 0.0481 1.0000 Uani C53 C -0.1931(4) 0.8790(4) 0.4824(2) 0.0591 1.0000 Uani C54 C -0.2993(4) 0.8934(4) 0.5205(3) 0.0608 1.0000 Uani C55 C -0.3278(3) 0.9015(4) 0.6065(3) 0.0602 1.0000 Uani C56 C -0.2504(3) 0.8955(3) 0.6569(2) 0.0477 1.0000 Uani C61 C -0.0682(2) 0.8261(3) 0.79277(18) 0.0364 1.0000 Uani C62 C -0.0315(3) 0.7092(3) 0.8155(2) 0.0457 1.0000 Uani C63 C -0.0430(3) 0.6602(3) 0.9008(2) 0.0577 1.0000 Uani C64 C -0.0913(3) 0.7272(3) 0.9645(2) 0.0551 1.0000 Uani C65 C -0.1299(3) 0.8436(3) 0.9424(2) 0.0546 1.0000 Uani C66 C -0.1193(3) 0.8942(3) 0.8568(2) 0.0468 1.0000 Uani C71 C -0.0837(2) 1.0339(3) 0.67686(18) 0.0379 1.0000 Uani C72 C -0.0233(3) 1.0589(3) 0.7253(2) 0.0447 1.0000 Uani C73 C -0.0429(3) 1.1698(3) 0.7186(2) 0.0512 1.0000 Uani C74 C -0.1238(3) 1.2577(3) 0.6661(3) 0.0576 1.0000 Uani C75 C -0.1858(3) 1.2350(3) 0.6200(2) 0.0558 1.0000 Uani C76 C -0.1646(3) 1.1225(3) 0.6244(2) 0.0434 1.0000 Uani C81 C 0.0945(2) 0.8127(3) 0.63834(17) 0.0380 1.0000 Uani C82 C 0.1695(3) 0.8598(3) 0.6283(2) 0.0470 1.0000 Uani C83 C 0.2839(3) 0.7951(4) 0.6029(2) 0.0587 1.0000 Uani C84 C 0.3224(3) 0.6880(4) 0.5871(2) 0.0567 1.0000 Uani C85 C 0.2486(3) 0.6409(3) 0.5949(2) 0.0535 1.0000 Uani C86 C 0.1336(3) 0.7041(3) 0.6209(2) 0.0458 1.0000 Uani H11 H 0.5774 0.1514 0.6117 0.0711(19) 1.0000 Uiso H12 H 0.4435 0.2148 0.5924 0.0711(19) 1.0000 Uiso H21 H 0.6462 0.0915 0.7947 0.0711(19) 1.0000 Uiso H22 H 0.5509 0.1459 0.8724 0.0711(19) 1.0000 Uiso H23 H 0.5864 0.2290 0.7943 0.0711(19) 1.0000 Uiso H121 H 0.8793 -0.6128 0.8526 0.0711(19) 1.0000 Uiso H131 H 0.9767 -0.8056 0.9276 0.0711(19) 1.0000 Uiso H141 H 0.8746 -0.9116 0.9918 0.0711(19) 1.0000 Uiso H151 H 0.6764 -0.8257 0.9874 0.0711(19) 1.0000 Uiso H161 H 0.5750 -0.6314 0.9192 0.0711(19) 1.0000 Uiso H221 H 0.8518 -0.4434 0.7616 0.0711(19) 1.0000 Uiso H231 H 0.9485 -0.4284 0.6209 0.0711(19) 1.0000 Uiso H241 H 0.8623 -0.4033 0.4961 0.0711(19) 1.0000 Uiso H251 H 0.6834 -0.4036 0.5087 0.0711(19) 1.0000 Uiso H261 H 0.5884 -0.4268 0.6490 0.0711(19) 1.0000 Uiso H321 H 0.6131 -0.2284 0.7838 0.0711(19) 1.0000 Uiso H331 H 0.6020 -0.1000 0.8695 0.0711(19) 1.0000 Uiso H341 H 0.6353 -0.1648 1.0182 0.0711(19) 1.0000 Uiso H351 H 0.6789 -0.3563 1.0844 0.0711(19) 1.0000 Uiso H361 H 0.6832 -0.4849 1.0026 0.0711(19) 1.0000 Uiso H421 H 0.4268 -0.2732 0.8659 0.0711(19) 1.0000 Uiso H431 H 0.2345 -0.2384 0.8623 0.0711(19) 1.0000 Uiso H441 H 0.1984 -0.3722 0.8172 0.0711(19) 1.0000 Uiso H451 H 0.3511 -0.5331 0.7618 0.0711(19) 1.0000 Uiso H461 H 0.5427 -0.5685 0.7625 0.0711(19) 1.0000 Uiso H521 H -0.0379 0.8638 0.5041 0.0711(19) 1.0000 Uiso H531 H -0.1729 0.8732 0.4192 0.0711(19) 1.0000 Uiso H541 H -0.3562 0.8983 0.4846 0.0711(19) 1.0000 Uiso H551 H -0.4047 0.9121 0.6333 0.0711(19) 1.0000 Uiso H561 H -0.2704 0.9001 0.7199 0.0711(19) 1.0000 Uiso H621 H 0.0047 0.6599 0.7698 0.0711(19) 1.0000 Uiso H631 H -0.0195 0.5767 0.9161 0.0711(19) 1.0000 Uiso H641 H -0.0961 0.6910 1.0268 0.0711(19) 1.0000 Uiso H651 H -0.1666 0.8920 0.9883 0.0711(19) 1.0000 Uiso H661 H -0.1471 0.9791 0.8411 0.0711(19) 1.0000 Uiso H721 H 0.0335 0.9960 0.7654 0.0711(19) 1.0000 Uiso H731 H 0.0018 1.1865 0.7525 0.0711(19) 1.0000 Uiso H741 H -0.1381 1.3385 0.6621 0.0711(19) 1.0000 Uiso H751 H -0.2461 1.2989 0.5831 0.0711(19) 1.0000 Uiso H761 H -0.2076 1.1057 0.5892 0.0711(19) 1.0000 Uiso H821 H 0.1408 0.9392 0.6396 0.0711(19) 1.0000 Uiso H831 H 0.3379 0.8284 0.5954 0.0711(19) 1.0000 Uiso H841 H 0.4050 0.6412 0.5697 0.0711(19) 1.0000 Uiso H851 H 0.2785 0.5619 0.5825 0.0711(19) 1.0000 Uiso H861 H 0.0796 0.6706 0.6267 0.0711(19) 1.0000 Uiso 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 0.03089(15) 0.03576(16) 0.04238(16) -0.0098(1) -0.0012(1) -0.01599(11) Mo2 0.03835(16) 0.03608(16) 0.04856(17) -0.00852(11) -0.00261(11) -0.01967(12) Si1 0.0280(4) 0.0416(4) 0.0504(5) -0.0140(3) 0.0025(3) -0.0165(3) P1 0.0340(4) 0.0411(4) 0.0391(4) -0.0091(3) -0.0027(3) -0.0201(3) P2 0.0347(4) 0.0371(4) 0.0340(3) -0.0098(3) -0.0005(3) -0.0187(3) Cl1 0.0678(6) 0.0701(6) 0.0717(6) -0.0068(5) 0.0190(5) -0.0353(5) O1 0.0682(16) 0.0542(14) 0.0595(15) 0.0039(11) -0.0078(12) -0.0337(13) O2 0.0402(12) 0.0508(13) 0.0638(14) -0.0297(11) 0.002(1) -0.012(1) O3 0.0331(11) 0.0612(15) 0.0793(17) -0.0245(13) 0.0026(11) -0.0144(11) O4 0.0497(13) 0.0552(14) 0.0653(15) -0.0084(11) -0.0195(11) -0.0270(11) O5 0.0504(12) 0.0514(13) 0.0458(12) -0.017(1) -0.0036(9) -0.0264(11) O6 0.029(1) 0.0444(11) 0.0569(12) -0.0193(9) 0.0035(8) -0.0198(9) O7 0.034(1) 0.0395(11) 0.0711(15) -0.018(1) 0.005(1) -0.0155(9) O8 0.037(1) 0.0478(12) 0.0441(11) -0.0137(9) 0.0034(8) -0.0223(9) O9 0.0423(12) 0.0545(14) 0.0673(15) -0.0114(11) 0.002(1) -0.0300(11) O10 0.0708(18) 0.0656(17) 0.098(2) -0.0315(16) -0.0113(15) -0.0408(15) O11 0.0741(18) 0.0653(17) 0.0784(19) -0.0401(15) 0.0050(14) -0.0308(15) O12 0.0582(15) 0.0521(15) 0.0722(17) 0.0076(12) -0.0081(12) -0.0244(12) C1 0.0516(19) 0.059(2) 0.058(2) -0.0189(16) 0.0118(15) -0.0233(17) C2 0.0429(18) 0.065(2) 0.083(3) -0.016(2) -0.0141(17) -0.0259(17) C11 0.0369(14) 0.0445(16) 0.0418(15) -0.0109(12) -0.0009(11) -0.0193(13) C12 0.0407(17) 0.059(2) 0.062(2) -0.0027(17) -0.0023(14) -0.0210(16) C13 0.050(2) 0.060(2) 0.068(2) -0.0080(19) -0.0071(17) -0.0083(18) C14 0.083(3) 0.048(2) 0.056(2) -0.0067(16) -0.0139(19) -0.0172(19) C15 0.081(3) 0.059(2) 0.065(2) 0.0031(18) -0.014(2) -0.041(2) C16 0.0542(19) 0.056(2) 0.0539(19) -0.0000(15) -0.0068(15) -0.0314(17) C21 0.0389(15) 0.0396(15) 0.0419(15) -0.0065(11) -0.0028(11) -0.0194(12) C22 0.0444(17) 0.058(2) 0.0487(17) -0.0049(14) -0.0047(13) -0.0274(15) C23 0.051(2) 0.066(2) 0.059(2) -0.0106(17) 0.0077(16) -0.0300(18) C24 0.071(2) 0.067(2) 0.0460(19) -0.0102(16) 0.0081(16) -0.033(2) C25 0.076(3) 0.073(3) 0.0439(18) -0.0106(17) -0.0075(17) -0.034(2) C26 0.0534(19) 0.061(2) 0.0477(18) -0.0090(15) -0.0075(14) -0.0285(16) C31 0.0342(13) 0.0478(16) 0.0418(15) -0.0117(12) -0.0019(11) -0.0223(12) C32 0.0511(18) 0.0471(17) 0.0489(17) -0.0086(14) -0.0079(14) -0.0241(15) C33 0.0543(19) 0.0491(19) 0.072(2) -0.0158(16) -0.0057(16) -0.0284(16) C34 0.059(2) 0.068(2) 0.067(2) -0.0338(19) 0.0047(17) -0.0384(19) C35 0.074(2) 0.081(3) 0.0490(19) -0.0183(18) -0.0084(17) -0.045(2) C36 0.061(2) 0.060(2) 0.0441(17) -0.0071(14) -0.0062(14) -0.0344(17) C41 0.0333(14) 0.0414(15) 0.0494(16) -0.0111(12) -0.0038(11) -0.0187(12) C42 0.0401(16) 0.0510(18) 0.063(2) -0.0216(15) -0.0009(14) -0.0192(14) C43 0.0364(17) 0.075(2) 0.066(2) -0.0220(19) -0.0006(15) -0.0207(17) C44 0.0416(17) 0.081(3) 0.0532(19) -0.0035(17) -0.0092(14) -0.0337(18) C45 0.058(2) 0.064(2) 0.0536(18) -0.0014(16) -0.0143(15) -0.0423(18) C46 0.0485(17) 0.0438(17) 0.0572(18) -0.0104(14) -0.0083(14) -0.0259(14) C51 0.0410(15) 0.0435(15) 0.0382(14) -0.0106(12) -0.0036(11) -0.0246(13) C52 0.0550(19) 0.062(2) 0.0390(15) -0.0129(14) 0.0002(13) -0.0357(17) C53 0.078(3) 0.074(2) 0.0424(17) -0.0119(16) -0.0112(16) -0.045(2) C54 0.066(2) 0.067(2) 0.068(2) -0.0093(18) -0.0259(18) -0.039(2) C55 0.0459(18) 0.070(2) 0.073(2) -0.0125(19) -0.0096(16) -0.0313(18) C56 0.0434(16) 0.0555(19) 0.0500(17) -0.0156(14) 0.0026(13) -0.0264(15) C61 0.0318(13) 0.0414(15) 0.0362(13) -0.0090(11) -0.000(1) -0.0168(12) C62 0.0450(16) 0.0449(16) 0.0447(16) -0.0120(13) 0.0069(13) -0.0203(14) C63 0.056(2) 0.0492(19) 0.0517(19) -0.0014(15) 0.0071(15) -0.0192(16) C64 0.0527(19) 0.065(2) 0.0408(16) -0.0020(15) 0.0021(14) -0.0265(17) C65 0.058(2) 0.065(2) 0.0406(16) -0.0199(15) 0.0060(14) -0.0267(18) C66 0.0508(17) 0.0481(17) 0.0418(16) -0.0121(13) -0.0012(13) -0.0219(15) C71 0.0352(14) 0.0431(15) 0.0387(14) -0.0111(12) 0.0014(11) -0.0203(12) C72 0.0424(16) 0.0480(17) 0.0517(17) -0.0129(13) -0.0066(13) -0.0242(14) C73 0.0483(18) 0.056(2) 0.064(2) -0.0229(16) 0.0015(15) -0.0317(16) C74 0.064(2) 0.0420(17) 0.070(2) -0.0145(16) 0.0027(17) -0.0275(16) C75 0.059(2) 0.0421(17) 0.056(2) -0.0041(14) -0.0075(16) -0.0158(16) C76 0.0397(15) 0.0458(17) 0.0450(16) -0.0092(13) -0.0043(12) -0.0189(13) C81 0.0382(14) 0.0446(15) 0.0328(13) -0.0081(11) 0.0013(11) -0.0210(12) C82 0.0431(16) 0.0527(18) 0.0511(17) -0.0163(14) 0.0059(13) -0.0265(15) C83 0.0417(17) 0.083(3) 0.056(2) -0.0162(18) 0.0072(14) -0.0344(18) C84 0.0382(16) 0.072(2) 0.0484(18) -0.0147(16) 0.0077(13) -0.0177(16) C85 0.0487(18) 0.0464(18) 0.0508(18) -0.0157(14) 0.0080(14) -0.0112(15) C86 0.0430(16) 0.0465(17) 0.0461(16) -0.0144(13) 0.0081(13) -0.0204(14) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source 'Mo ' -1.6832 0.6857 3.7025 0.2772 17.2356 1.0958 12.8876 11.0040 3.7429 61.6584 4.3875 International_Tables_Vol_IV_Table_2.2B 'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 International_Tables_Vol_IV_Table_2.2B 'P ' 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645 1.1149 International_Tables_Vol_IV_Table_2.2B 'Si ' 0.0817 0.0704 6.2915 2.4386 3.0353 32.3337 1.9891 0.6785 1.5410 81.6937 1.1407 International_Tables_Vol_IV_Table_2.2B 'Cl ' 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784 -9.5574 International_Tables_Vol_IV_Table_2.2B 'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 International_Tables_Vol_IV_Table_2.2B 'O ' 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 International_Tables_Vol_IV_Table_2.2B loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O1 Mo1 O2 104.01(13) yes O1 Mo1 O3 103.58(13) yes O2 Mo1 O3 44.76(11) yes O1 Mo1 O4 98.50(13) yes O2 Mo1 O4 131.17(11) yes O3 Mo1 O4 88.16(12) yes O1 Mo1 O5 102.11(12) yes O2 Mo1 O5 153.87(11) yes O3 Mo1 O5 128.31(11) yes O4 Mo1 O5 44.0(1) yes O1 Mo1 O6 99.33(12) yes O2 Mo1 O6 85.49(9) yes O3 Mo1 O6 128.75(11) yes O4 Mo1 O6 132.7(1) yes O5 Mo1 O6 89.44(9) yes O1 Mo1 O8 170.71(11) yes O2 Mo1 O8 82.2(1) yes O3 Mo1 O8 85.7(1) yes O4 Mo1 O8 82.07(9) yes O5 Mo1 O8 71.81(8) yes O6 Mo1 O8 73.98(8) yes O5 Mo2 O7 76.09(9) yes O5 Mo2 O8 70.44(8) yes O7 Mo2 O8 89.99(9) yes O5 Mo2 O9 80.43(9) yes O7 Mo2 O9 133.4(1) yes O8 Mo2 O9 44.02(9) yes O5 Mo2 O10 85.15(11) yes O7 Mo2 O10 130.05(12) yes O8 Mo2 O10 126.54(11) yes O9 Mo2 O10 86.43(12) yes O5 Mo2 O11 81.97(11) yes O7 Mo2 O11 86.09(12) yes O8 Mo2 O11 152.25(12) yes O9 Mo2 O11 129.60(12) yes O10 Mo2 O11 45.20(13) yes O5 Mo2 O12 170.83(12) yes O7 Mo2 O12 98.06(12) yes O8 Mo2 O12 102.84(13) yes O9 Mo2 O12 99.18(13) yes O10 Mo2 O12 103.99(15) yes O11 Mo2 O12 104.91(15) yes O6 Si1 O7 111.46(11) yes O6 Si1 C1 107.07(15) yes O7 Si1 C1 108.05(16) yes O6 Si1 C2 110.10(16) yes O7 Si1 C2 110.41(17) yes C1 Si1 C2 109.66(19) yes C11 P1 C21 110.86(14) yes C11 P1 C31 109.06(14) yes C21 P1 C31 108.72(14) yes C11 P1 C41 108.33(14) yes C21 P1 C41 109.90(14) yes C31 P1 C41 109.96(14) yes C51 P2 C61 109.34(13) yes C51 P2 C71 109.37(14) yes C61 P2 C71 108.57(13) yes C51 P2 C81 109.78(14) yes C61 P2 C81 110.53(13) yes C71 P2 C81 109.23(14) yes Mo1 O2 O3 67.63(14) yes Mo1 O3 O2 67.60(13) yes Mo1 O4 O5 71.13(12) yes Mo1 O5 Mo2 107.26(9) yes Mo1 O5 O4 64.89(13) yes Mo2 O5 O4 111.39(16) yes Mo1 O6 Si1 129.76(12) yes Mo2 O7 Si1 134.82(13) yes Mo1 O8 Mo2 108.99(9) yes Mo1 O8 O9 111.10(15) yes Mo2 O8 O9 65.32(13) yes Mo2 O9 O8 70.66(12) yes Mo2 O10 O11 67.88(15) yes Mo2 O11 O10 66.92(15) yes Si1 C1 Cl1 108.7(2) yes Si1 C1 H11 109.022 no Cl1 C1 H11 109.936 no Si1 C1 H12 109.279 no Cl1 C1 H12 110.255 no H11 C1 H12 109.582 no Si1 C2 H21 110.193 no Si1 C2 H22 109.642 no H21 C2 H22 109.185 no Si1 C2 H23 109.803 no H21 C2 H23 109.385 no H22 C2 H23 108.604 no P1 C11 C12 119.4(3) yes P1 C11 C16 121.7(3) yes C12 C11 C16 118.8(3) yes C11 C12 C13 119.7(4) yes C11 C12 H121 120.139 no C13 C12 H121 120.180 no C12 C13 C14 120.4(4) yes C12 C13 H131 120.232 no C14 C13 H131 119.404 no C13 C14 C15 120.2(4) yes C13 C14 H141 120.211 no C15 C14 H141 119.564 no C14 C15 C16 120.1(4) yes C14 C15 H151 119.134 no C16 C15 H151 120.736 no C11 C16 C15 120.7(3) yes C11 C16 H161 120.278 no C15 C16 H161 119.004 no P1 C21 C22 119.7(2) yes P1 C21 C26 121.3(2) yes C22 C21 C26 119.0(3) yes C21 C22 C23 120.2(3) yes C21 C22 H221 119.466 no C23 C22 H221 120.290 no C22 C23 C24 120.3(4) yes C22 C23 H231 120.153 no C24 C23 H231 119.511 no C23 C24 C25 120.1(3) yes C23 C24 H241 119.211 no C25 C24 H241 120.631 no C24 C25 C26 120.4(4) yes C24 C25 H251 119.961 no C26 C25 H251 119.628 no C21 C26 C25 119.8(3) yes C21 C26 H261 120.129 no C25 C26 H261 120.022 no P1 C31 C32 119.2(2) yes P1 C31 C36 120.7(3) yes C32 C31 C36 120.1(3) yes C31 C32 C33 119.5(3) yes C31 C32 H321 120.514 no C33 C32 H321 119.997 no C32 C33 C34 120.2(3) yes C32 C33 H331 120.216 no C34 C33 H331 119.627 no C33 C34 C35 120.3(3) yes C33 C34 H341 119.717 no C35 C34 H341 120.028 no C34 C35 C36 120.5(3) yes C34 C35 H351 119.168 no C36 C35 H351 120.290 no C31 C36 C35 119.5(3) yes C31 C36 H361 120.522 no C35 C36 H361 119.991 no P1 C41 C42 119.7(2) yes P1 C41 C46 119.8(2) yes C42 C41 C46 120.5(3) yes C41 C42 C43 118.1(3) yes C41 C42 H421 121.164 no C43 C42 H421 120.719 no C42 C43 C44 120.8(3) yes C42 C43 H431 119.479 no C44 C43 H431 119.738 no C43 C44 C45 120.5(3) yes C43 C44 H441 119.550 no C45 C44 H441 119.893 no C44 C45 C46 119.9(3) yes C44 C45 H451 119.927 no C46 C45 H451 120.206 no C41 C46 C45 120.1(3) yes C41 C46 H461 119.587 no C45 C46 H461 120.331 no P2 C51 C52 120.3(2) yes P2 C51 C56 119.1(2) yes C52 C51 C56 120.4(3) yes C51 C52 C53 119.4(3) yes C51 C52 H521 120.264 no C53 C52 H521 120.311 no C52 C53 C54 119.8(3) yes C52 C53 H531 120.031 no C54 C53 H531 120.127 no C53 C54 C55 120.6(3) yes C53 C54 H541 119.682 no C55 C54 H541 119.673 no C54 C55 C56 120.3(3) yes C54 C55 H551 120.062 no C56 C55 H551 119.596 no C51 C56 C55 119.3(3) yes C51 C56 H561 120.008 no C55 C56 H561 120.692 no P2 C61 C62 119.8(2) yes P2 C61 C66 120.8(2) yes C62 C61 C66 119.4(3) yes C61 C62 C63 120.3(3) yes C61 C62 H621 119.834 no C63 C62 H621 119.811 no C62 C63 C64 120.3(3) yes C62 C63 H631 119.699 no C64 C63 H631 119.932 no C63 C64 C65 119.8(3) yes C63 C64 H641 120.267 no C65 C64 H641 119.932 no C64 C65 C66 120.6(3) yes C64 C65 H651 119.617 no C66 C65 H651 119.827 no C61 C66 C65 119.6(3) yes C61 C66 H661 120.117 no C65 C66 H661 120.266 no P2 C71 C72 119.1(2) yes P2 C71 C76 121.6(2) yes C72 C71 C76 119.3(3) yes C71 C72 C73 120.2(3) yes C71 C72 H721 120.358 no C73 C72 H721 119.400 no C72 C73 C74 120.0(3) yes C72 C73 H731 119.623 no C74 C73 H731 120.337 no C73 C74 C75 120.4(3) yes C73 C74 H741 119.525 no C75 C74 H741 120.029 no C74 C75 C76 120.0(3) yes C74 C75 H751 120.520 no C76 C75 H751 119.490 no C71 C76 C75 120.0(3) yes C71 C76 H761 119.964 no C75 C76 H761 120.050 no P2 C81 C82 120.2(2) yes P2 C81 C86 119.7(2) yes C82 C81 C86 120.0(3) yes C81 C82 C83 119.4(3) yes C81 C82 H821 120.041 no C83 C82 H821 120.534 no C82 C83 C84 120.4(3) yes C82 C83 H831 119.815 no C84 C83 H831 119.730 no C83 C84 C85 120.8(3) yes C83 C84 H841 120.255 no C85 C84 H841 118.897 no C84 C85 C86 119.5(3) yes C84 C85 H851 119.691 no C86 C85 H851 120.758 no C81 C86 C85 119.8(3) yes C81 C86 H861 120.216 no C85 C86 H861 120.025 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Mo1 O1 1.683(3) yes Mo1 O2 1.925(2) yes Mo1 O3 1.925(2) yes Mo1 O4 1.910(2) yes Mo1 O5 1.996(2) yes Mo1 O6 1.961(2) yes Mo1 O8 2.430(2) yes Mo2 O5 2.485(2) yes Mo2 O7 1.958(2) yes Mo2 O8 2.006(2) yes Mo2 O9 1.932(2) yes Mo2 O10 1.913(3) yes Mo2 O11 1.926(3) yes Mo2 O12 1.678(3) yes Si1 O6 1.613(2) yes Si1 O7 1.612(2) yes Si1 C1 1.875(4) yes Si1 C2 1.857(4) yes P1 C11 1.799(3) yes P1 C21 1.797(3) yes P1 C31 1.787(3) yes P1 C41 1.797(3) yes P2 C51 1.797(3) yes P2 C61 1.796(3) yes P2 C71 1.783(3) yes P2 C81 1.799(3) yes Cl1 C1 1.808(4) yes O2 O3 1.466(4) yes O4 O5 1.465(3) yes O8 O9 1.477(3) yes O10 O11 1.476(4) yes C1 H11 1.002 no C1 H12 0.996 no C2 H21 0.997 no C2 H22 1.007 no C2 H23 1.004 no C11 C12 1.397(5) yes C11 C16 1.393(5) yes C12 C13 1.388(6) yes C12 H121 1.003 no C13 C14 1.385(7) yes C13 H131 1.002 no C14 C15 1.365(7) yes C14 H141 1.004 no C15 C16 1.382(5) yes C15 H151 1.004 no C16 H161 1.003 no C21 C22 1.401(4) yes C21 C26 1.387(5) yes C22 C23 1.378(5) yes C22 H221 1.008 no C23 C24 1.376(6) yes C23 H231 1.006 no C24 C25 1.372(6) yes C24 H241 0.997 no C25 C26 1.393(5) yes C25 H251 1.006 no C26 H261 1.004 no C31 C32 1.394(5) yes C31 C36 1.388(4) yes C32 C33 1.386(5) yes C32 H321 1.004 no C33 C34 1.372(6) yes C33 H331 1.005 no C34 C35 1.380(6) yes C34 H341 1.000 no C35 C36 1.377(5) yes C35 H351 1.008 no C36 H361 1.010 no C41 C42 1.395(5) yes C41 C46 1.396(4) yes C42 C43 1.398(5) yes C42 H421 1.004 no C43 C44 1.376(6) yes C43 H431 1.010 no C44 C45 1.381(6) yes C44 H441 1.008 no C45 C46 1.372(5) yes C45 H451 1.008 no C46 H461 1.008 no C51 C52 1.394(4) yes C51 C56 1.386(4) yes C52 C53 1.385(5) yes C52 H521 1.010 no C53 C54 1.385(6) yes C53 H531 1.007 no C54 C55 1.369(6) yes C54 H541 1.006 no C55 C56 1.390(5) yes C55 H551 0.999 no C56 H561 1.000 no C61 C62 1.385(4) yes C61 C66 1.396(4) yes C62 C63 1.377(5) yes C62 H621 1.003 no C63 C64 1.382(6) yes C63 H631 0.995 no C64 C65 1.375(6) yes C64 H641 1.000 no C65 C66 1.385(5) yes C65 H651 0.997 no C66 H661 1.004 no C71 C72 1.411(4) yes C71 C76 1.385(4) yes C72 C73 1.376(5) yes C72 H721 1.005 no C73 C74 1.382(6) yes C73 H731 1.007 no C74 C75 1.384(6) yes C74 H741 1.004 no C75 C76 1.394(5) yes C75 H751 1.003 no C76 H761 1.006 no C81 C82 1.402(4) yes C81 C86 1.383(4) yes C82 C83 1.395(5) yes C82 H821 1.003 no C83 C84 1.358(6) yes C83 H831 1.002 no C84 C85 1.392(6) yes C84 H841 1.004 no C85 C86 1.399(5) yes C85 H851 1.002 no C86 H861 1.010 no