#------------------------------------------------------------------------------ #$Date: 2019-10-28 07:23:29 +0000 (Mon, 28 Oct 2019) $ #$Revision: 219800 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/30/2003087.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2003087 loop_ _publ_author_name 'Krebs, Frederik C.' 'Laursen, Bo W.' 'Johannsen, Ib' 'Faldt, Andr\'e' 'Bechgaard, Klaus' 'Jacobsen, Claus S.' 'Thorup, Niels' 'Boubekeur, Kamal' _publ_section_title ; The geometry and structural properties of the 4,8,12-trioxa-4,8,12,12c-tetrahydrodibenzo[cd,mn]pyrene system in the cationic state. Structures of a planar organic cation with various monovalent and divalent anions ; _journal_coden_ASTM ASBSDK _journal_issue 3 _journal_name_full ; Acta Crystallographica, Section B: Structural Science ; _journal_page_first 410 _journal_page_last 423 _journal_paper_doi 10.1107/S0108768198016140 _journal_volume 55 _journal_year 1999 _chemical_formula_moiety '2(C31 H33 O3), Cl14 Mo6' _chemical_formula_sum 'C62 H66 Cl14 Mo6 O6' _chemical_formula_weight 1979.08 _chemical_name_systematic ; Bis(2,6,10-tri-tert-butyl-4,8,12-trioxa-4,8,12,12c-tetrahydro- dibenzo[cd,mn]pyrenium) tetradecachlorohexamolybdate ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 96.40(3) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 17.157(3) _cell_length_b 11.130(2) _cell_length_c 18.456(4) _cell_measurement_temperature 120(2) _cell_volume 3502.3(12) _computing_cell_refinement 'SAINT Siemens' _computing_data_collection 'SMART Siemens' _computing_data_reduction 'SAINT Siemens' _computing_molecular_graphics 'SHELXTL (Sheldrick)' _computing_publication_material 'XCIF (Sheldrick)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.948 _diffrn_measured_fraction_theta_max 0.948 _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method 'omega scan, frame data integration' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0271 _diffrn_reflns_av_sigmaI/netI 0.0197 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 36072 _diffrn_reflns_theta_full 26.37 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_min 1.54 _exptl_absorpt_coefficient_mu 1.624 _exptl_absorpt_correction_T_max 0.886 _exptl_absorpt_correction_T_min 0.704 _exptl_absorpt_correction_type empirical _exptl_crystal_colour orange _exptl_crystal_density_diffrn 1.877 _exptl_crystal_density_method 'not measured' _exptl_crystal_description cube _exptl_crystal_F_000 1952 _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _refine_diff_density_max 0.434 _refine_diff_density_min -1.313 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 397 _refine_ls_number_reflns 7149 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.097 _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0234 _refine_ls_shift/su_max 0.005 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+1.6569P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref 0.0582 _reflns_number_gt 6258 _reflns_number_total 7149 _reflns_threshold_expression >2sigma(I) _cod_data_source_file os0007.cif _cod_data_source_block 12 _cod_depositor_comments ; The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+1.6569P] where P=(Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+1.6569P] where P=(Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 2019-10-23 Z value and formula fixed to values more according to usual chemical conventions. miguel ; _cod_original_formula_sum 'C31 H33 Cl7 Mo3 O3' _cod_original_formula_weight 989.54 _cod_original_formula_moiety 'C31 H33 O3,Cl7 Mo3' _cod_original_formula_units_Z 4 _cod_original_cell_volume 3502.4(12) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2003087 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _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 _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Mo1 0.950784(10) 0.876155(17) 0.043899(10) 0.01156(5) Uani d . 1 . . Mo Mo2 1.014830(10) 1.079316(17) 0.088032(10) 0.01214(5) Uani d . 1 . . Mo Mo3 1.095215(10) 0.923207(17) 0.021136(10) 0.01187(5) Uani d . 1 . . Mo Cl1 0.88433(3) 0.71653(5) 0.10371(3) 0.02044(12) Uani d . 1 . . Cl Cl2 1.03377(4) 1.17836(6) 0.20545(3) 0.02654(14) Uani d . 1 . . Cl Cl3 1.22017(3) 0.81908(5) 0.04631(3) 0.02215(13) Uani d . 1 . . Cl Cl4 0.87735(3) 1.03036(5) 0.10448(3) 0.01702(12) Uani d . 1 . . Cl Cl5 1.15006(3) 1.12096(5) 0.06237(3) 0.01617(11) Uani d . 1 . . Cl Cl6 1.02882(3) 0.73467(5) -0.02202(3) 0.01627(11) Uani d . 1 . . Cl Cl7 1.05821(3) 0.88635(5) 0.14517(3) 0.01713(11) Uani d . 1 . . Cl O1 0.45707(8) 0.82772(14) -0.15806(8) 0.0135(3) Uani d . 1 . . O O2 0.31766(8) 1.08819(14) -0.00779(8) 0.0139(3) Uani d . 1 . . O O3 0.49862(8) 0.79292(14) 0.10404(8) 0.0143(3) Uani d . 1 . . O C1 0.42274(12) 0.90108(19) -0.02062(12) 0.0116(4) Uani d . 1 . . C C2 0.38625(12) 0.9570(2) -0.08306(12) 0.0126(4) Uani d . 1 . . C C3 0.40530(12) 0.92167(19) -0.15203(12) 0.0130(4) Uani d . 1 . . C C4 0.37376(12) 0.9821(2) -0.21344(11) 0.0140(4) Uani d . 1 . . C H4 0.3863 0.9595 -0.2592 0.017 Uiso calc . 1 . . H C5 0.32230(12) 1.0787(2) -0.20608(12) 0.0136(4) Uani d . 1 . . C C6 0.30081(12) 1.1120(2) -0.13717(12) 0.0147(4) Uani d . 1 . . C H6 0.2648 1.1734 -0.1331 0.018 Uiso calc . 1 . . H C7 0.33425(12) 1.0517(2) -0.07596(12) 0.0132(4) Uani d . 1 . . C C8 0.40717(12) 0.93901(19) 0.04778(12) 0.0121(4) Uani d . 1 . . C C9 0.35416(12) 1.0337(2) 0.05407(12) 0.0130(4) Uani d . 1 . . C C10 0.33960(12) 1.07279(19) 0.12195(12) 0.0137(4) Uani d . 1 . . C H10 0.3059 1.1371 0.1264 0.016 Uiso calc . 1 . . H C11 0.37588(12) 1.01525(19) 0.18422(12) 0.0128(4) Uani d . 1 . . C C12 0.42924(12) 0.9201(2) 0.17862(12) 0.0137(4) Uani d . 1 . . C H12 0.4534 0.8827 0.2203 0.016 Uiso calc . 1 . . H C13 0.44492(12) 0.88392(19) 0.11086(12) 0.0124(4) Uani d . 1 . . C C14 0.47708(12) 0.80968(19) -0.02700(11) 0.0125(4) Uani d . 1 . . C C15 0.51501(12) 0.75612(19) 0.03610(11) 0.0123(4) Uani d . 1 . . C C16 0.56837(12) 0.6654(2) 0.02997(12) 0.0138(4) Uani d . 1 . . C H16 0.5941 0.6300 0.0716 0.017 Uiso calc . 1 . . H C17 0.58391(12) 0.62647(19) -0.03938(12) 0.0134(4) Uani d . 1 . . C C18 0.54567(12) 0.6798(2) -0.10273(12) 0.0137(4) Uani d . 1 . . C H18 0.5557 0.6531 -0.1485 0.016 Uiso calc . 1 . . H C19 0.49324(12) 0.7719(2) -0.09639(11) 0.0127(4) Uani d . 1 . . C C20 0.28787(13) 1.1522(2) -0.27219(12) 0.0168(5) Uani d . 1 . . C C21 0.19862(14) 1.1307(2) -0.28355(13) 0.0215(5) Uani d . 1 . . C H21A 0.1763 1.1509 -0.2397 0.032 Uiso calc . 1 . . H H21B 0.1885 1.0476 -0.2951 0.032 Uiso calc . 1 . . H H21C 0.1756 1.1800 -0.3229 0.032 Uiso calc . 1 . . H C22 0.32445(14) 1.1189(2) -0.34166(13) 0.0232(5) Uani d . 1 . . C H22A 0.3800 1.1323 -0.3341 0.035 Uiso calc . 1 . . H H22B 0.3018 1.1677 -0.3814 0.035 Uiso calc . 1 . . H H22C 0.3144 1.0357 -0.3529 0.035 Uiso calc . 1 . . H C23 0.30369(15) 1.2866(2) -0.25642(13) 0.0236(5) Uani d . 1 . . C H23A 0.3592 1.3005 -0.2491 0.035 Uiso calc . 1 . . H H23B 0.2807 1.3095 -0.2134 0.035 Uiso calc . 1 . . H H23C 0.2810 1.3336 -0.2970 0.035 Uiso calc . 1 . . H C24 0.35515(13) 1.0489(2) 0.26010(12) 0.0171(5) Uani d . 1 . . C C25 0.30681(14) 1.1646(2) 0.25967(13) 0.0229(5) Uani d . 1 . . C H25A 0.2602 1.1562 0.2261 0.034 Uiso calc . 1 . . H H25B 0.3374 1.2307 0.2450 0.034 Uiso calc . 1 . . H H25C 0.2925 1.1794 0.3077 0.034 Uiso calc . 1 . . H C26 0.43001(16) 1.0650(3) 0.31308(14) 0.0298(6) Uani d . 1 . . C H26A 0.4161 1.0855 0.3605 0.045 Uiso calc . 1 . . H H26B 0.4613 1.1281 0.2958 0.045 Uiso calc . 1 . . H H26C 0.4594 0.9914 0.3160 0.045 Uiso calc . 1 . . H C27 0.30638(18) 0.9441(3) 0.28503(16) 0.0346(7) Uani d . 1 . . C H27A 0.2600 0.9342 0.2514 0.052 Uiso calc . 1 . . H H27B 0.2918 0.9609 0.3327 0.052 Uiso calc . 1 . . H H27C 0.3369 0.8716 0.2866 0.052 Uiso calc . 1 . . H C28 0.64667(12) 0.5300(2) -0.04476(12) 0.0143(4) Uani d . 1 . . C C29 0.63263(14) 0.4595(2) -0.11678(13) 0.0203(5) Uani d . 1 . . C H29A 0.6328 0.5140 -0.1571 0.031 Uiso calc . 1 . . H H29B 0.5828 0.4195 -0.1195 0.031 Uiso calc . 1 . . H H29C 0.6735 0.4010 -0.1187 0.031 Uiso calc . 1 . . H C30 0.72640(14) 0.5947(2) -0.03938(14) 0.0228(5) Uani d . 1 . . C H30A 0.7344 0.6384 0.0057 0.034 Uiso calc . 1 . . H H30B 0.7270 0.6495 -0.0795 0.034 Uiso calc . 1 . . H H30C 0.7675 0.5366 -0.0410 0.034 Uiso calc . 1 . . H C31 0.64836(14) 0.4411(2) 0.01860(14) 0.0219(5) Uani d . 1 . . C H31A 0.6552 0.4841 0.0639 0.033 Uiso calc . 1 . . H H31B 0.6911 0.3860 0.0166 0.033 Uiso calc . 1 . . H H31C 0.5999 0.3973 0.0150 0.033 Uiso calc . 1 . . H 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 Mo1 0.01039(9) 0.01106(10) 0.01335(10) -0.00042(7) 0.00189(7) -0.00083(7) Mo2 0.01238(9) 0.01202(10) 0.01198(10) -0.00028(7) 0.00120(7) -0.00290(7) Mo3 0.00936(9) 0.01110(10) 0.01507(10) 0.00076(7) 0.00105(7) -0.00121(7) Cl1 0.0187(3) 0.0178(3) 0.0252(3) -0.0031(2) 0.0044(2) 0.0046(2) Cl2 0.0354(3) 0.0265(3) 0.0173(3) -0.0032(3) 0.0011(2) -0.0103(2) Cl3 0.0127(2) 0.0180(3) 0.0352(3) 0.0039(2) 0.0003(2) 0.0011(2) Cl4 0.0158(3) 0.0175(3) 0.0190(3) 0.0003(2) 0.0074(2) -0.0028(2) Cl5 0.0120(2) 0.0156(3) 0.0203(3) -0.00195(19) -0.0012(2) -0.0021(2) Cl6 0.0158(2) 0.0117(3) 0.0215(3) 0.0010(2) 0.0030(2) -0.0031(2) Cl7 0.0182(3) 0.0174(3) 0.0150(3) 0.0000(2) -0.0013(2) 0.0017(2) O1 0.0156(7) 0.0132(8) 0.0118(7) 0.0033(6) 0.0023(6) 0.0004(6) O2 0.0133(7) 0.0150(8) 0.0137(8) 0.0036(6) 0.0032(6) 0.0012(6) O3 0.0161(7) 0.0145(8) 0.0126(7) 0.0042(6) 0.0032(6) 0.0008(6) C1 0.0097(9) 0.0091(10) 0.0162(11) -0.0030(8) 0.0027(8) -0.0001(8) C2 0.0105(10) 0.0121(11) 0.0154(11) -0.0002(8) 0.0021(8) 0.0020(8) C3 0.0103(10) 0.0118(11) 0.0169(11) -0.0009(8) 0.0022(8) 0.0000(9) C4 0.0139(10) 0.0162(12) 0.0121(10) -0.0013(9) 0.0028(8) -0.0003(9) C5 0.0114(10) 0.0131(11) 0.0161(11) -0.0019(8) 0.0012(8) 0.0023(9) C6 0.0125(10) 0.0127(11) 0.0190(11) 0.0019(8) 0.0028(9) 0.0015(9) C7 0.0110(10) 0.0143(11) 0.0144(11) -0.0019(8) 0.0027(8) -0.0011(9) C8 0.0112(10) 0.0113(11) 0.0143(11) -0.0015(8) 0.0033(8) 0.0002(8) C9 0.0113(10) 0.0130(11) 0.0146(11) -0.0015(8) 0.0016(8) 0.0016(9) C10 0.0103(10) 0.0127(11) 0.0184(11) -0.0018(8) 0.0035(8) -0.0027(9) C11 0.0115(10) 0.0123(11) 0.0154(11) -0.0053(8) 0.0048(8) -0.0032(9) C12 0.0147(10) 0.0134(11) 0.0130(11) -0.0020(8) 0.0013(8) 0.0022(9) C13 0.0115(10) 0.0091(11) 0.0171(11) 0.0007(8) 0.0034(8) 0.0016(8) C14 0.0119(10) 0.0103(10) 0.0159(11) -0.0012(8) 0.0039(8) -0.0013(8) C15 0.0121(10) 0.0118(11) 0.0136(10) -0.0010(8) 0.0040(8) -0.0012(8) C16 0.0146(10) 0.0127(11) 0.0139(10) 0.0010(8) 0.0004(8) 0.0020(9) C17 0.0114(10) 0.0105(11) 0.0189(11) -0.0021(8) 0.0042(8) -0.0003(9) C18 0.0141(10) 0.0135(11) 0.0142(10) -0.0017(8) 0.0043(8) -0.0013(9) C19 0.0112(10) 0.0123(11) 0.0149(11) -0.0013(8) 0.0034(8) 0.0027(8) C20 0.0176(11) 0.0172(12) 0.0156(11) 0.0029(9) 0.0016(9) 0.0040(9) C21 0.0189(11) 0.0254(13) 0.0196(12) 0.0044(10) -0.0012(9) 0.0028(10) C22 0.0258(13) 0.0279(14) 0.0164(12) 0.0089(10) 0.0045(10) 0.0060(10) C23 0.0294(13) 0.0188(13) 0.0230(13) 0.0021(10) 0.0045(10) 0.0064(10) C24 0.0198(11) 0.0175(12) 0.0148(11) 0.0011(9) 0.0057(9) -0.0022(9) C25 0.0251(12) 0.0258(14) 0.0183(12) 0.0067(10) 0.0046(10) -0.0060(10) C26 0.0329(14) 0.0376(16) 0.0172(12) 0.0143(12) -0.0046(11) -0.0106(11) C27 0.0465(17) 0.0268(15) 0.0362(16) -0.0020(12) 0.0301(13) 0.0022(12) C28 0.0131(10) 0.0135(11) 0.0163(11) 0.0019(9) 0.0023(8) -0.0015(9) C29 0.0212(11) 0.0178(12) 0.0220(12) 0.0061(10) 0.0023(9) -0.0040(10) C30 0.0147(11) 0.0234(13) 0.0313(14) -0.0009(10) 0.0064(10) -0.0058(11) C31 0.0251(12) 0.0162(12) 0.0255(13) 0.0073(10) 0.0073(10) 0.0025(10) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle Cl1 Mo1 Cl5 . 3_775 92.72(2) Cl1 Mo1 Cl4 . . 90.77(3) Cl5 Mo1 Cl4 3_775 . 90.17(2) Cl1 Mo1 Cl6 . . 93.72(3) Cl5 Mo1 Cl6 3_775 . 89.28(2) Cl4 Mo1 Cl6 . . 175.499(19) Cl1 Mo1 Cl7 . . 92.17(2) Cl5 Mo1 Cl7 3_775 . 175.10(2) Cl4 Mo1 Cl7 . . 90.05(2) Cl6 Mo1 Cl7 . . 90.13(2) Cl1 Mo1 Mo2 . . 133.837(19) Cl5 Mo1 Mo2 3_775 . 118.124(18) Cl4 Mo1 Mo2 . . 58.250(18) Cl6 Mo1 Mo2 . . 118.294(19) Cl7 Mo1 Mo2 . . 58.113(16) Cl1 Mo1 Mo3 . . 135.900(19) Cl5 Mo1 Mo3 3_775 . 117.61(2) Cl4 Mo1 Mo3 . . 118.33(2) Cl6 Mo1 Mo3 . . 58.21(2) Cl7 Mo1 Mo3 . . 58.18(2) Mo2 Mo1 Mo3 . . 60.102(11) Cl1 Mo1 Mo3 . 3_775 134.185(19) Cl5 Mo1 Mo3 3_775 3_775 58.324(16) Cl4 Mo1 Mo3 . 3_775 58.078(19) Cl6 Mo1 Mo3 . 3_775 118.04(2) Cl7 Mo1 Mo3 . 3_775 117.925(19) Mo2 Mo1 Mo3 . 3_775 59.83(2) Mo3 Mo1 Mo3 . 3_775 89.892(16) Cl1 Mo1 Mo2 . 3_775 136.404(19) Cl5 Mo1 Mo2 3_775 3_775 57.89(2) Cl4 Mo1 Mo2 . 3_775 117.98(2) Cl6 Mo1 Mo2 . 3_775 58.14(2) Cl7 Mo1 Mo2 . 3_775 117.88(2) Mo2 Mo1 Mo2 . 3_775 89.745(14) Mo3 Mo1 Mo2 . 3_775 59.73(3) Mo3 Mo1 Mo2 3_775 3_775 59.919(12) Cl2 Mo2 Cl5 . . 92.93(3) Cl2 Mo2 Cl7 . . 90.56(3) Cl5 Mo2 Cl7 . . 90.01(2) Cl2 Mo2 Cl4 . . 91.44(3) Cl5 Mo2 Cl4 . . 175.623(19) Cl7 Mo2 Cl4 . . 90.12(2) Cl2 Mo2 Cl6 . 3_775 93.60(3) Cl5 Mo2 Cl6 . 3_775 89.30(2) Cl7 Mo2 Cl6 . 3_775 175.811(19) Cl4 Mo2 Cl6 . 3_775 90.25(2) Cl2 Mo2 Mo3 . 3_775 135.33(2) Cl5 Mo2 Mo3 . 3_775 118.07(2) Cl7 Mo2 Mo3 . 3_775 118.618(18) Cl4 Mo2 Mo3 . 3_775 58.20(2) Cl6 Mo2 Mo3 3_775 3_775 58.302(17) Cl2 Mo2 Mo1 . . 133.25(2) Cl5 Mo2 Mo1 . . 118.477(17) Cl7 Mo2 Mo1 . . 58.35(2) Cl4 Mo2 Mo1 . . 58.132(16) Cl6 Mo2 Mo1 3_775 . 118.57(2) Mo3 Mo2 Mo1 3_775 . 60.284(11) Cl2 Mo2 Mo3 . . 134.48(2) Cl5 Mo2 Mo3 . . 58.40(2) Cl7 Mo2 Mo3 . . 58.249(18) Cl4 Mo2 Mo3 . . 118.20(2) Cl6 Mo2 Mo3 3_775 . 118.05(2) Mo3 Mo2 Mo3 3_775 . 90.145(15) Mo1 Mo2 Mo3 . . 60.090(14) Cl2 Mo2 Mo1 . 3_775 136.49(2) Cl5 Mo2 Mo1 . 3_775 58.02(3) Cl7 Mo2 Mo1 . 3_775 118.266(17) Cl4 Mo2 Mo1 . 3_775 118.25(3) Cl6 Mo2 Mo1 3_775 3_775 58.037(16) Mo3 Mo2 Mo1 3_775 3_775 60.061(18) Mo1 Mo2 Mo1 . 3_775 90.254(15) Mo3 Mo2 Mo1 . 3_775 60.026(17) Cl3 Mo3 Cl4 . 3_775 91.30(3) Cl3 Mo3 Cl6 . . 91.24(3) Cl4 Mo3 Cl6 3_775 . 90.25(2) Cl3 Mo3 Cl7 . . 93.20(3) Cl4 Mo3 Cl7 3_775 . 175.481(19) Cl6 Mo3 Cl7 . . 90.05(2) Cl3 Mo3 Cl5 . . 93.90(2) Cl4 Mo3 Cl5 3_775 . 89.82(2) Cl6 Mo3 Cl5 . . 174.856(18) Cl7 Mo3 Cl5 . . 89.48(2) Cl3 Mo3 Mo2 . 3_775 133.59(2) Cl4 Mo3 Mo2 3_775 3_775 58.24(2) Cl6 Mo3 Mo2 . 3_775 58.267(17) Cl7 Mo3 Mo2 . 3_775 118.36(2) Cl5 Mo3 Mo2 . 3_775 117.694(17) Cl3 Mo3 Mo1 . . 134.789(19) Cl4 Mo3 Mo1 3_775 . 118.43(3) Cl6 Mo3 Mo1 . . 58.078(16) Cl7 Mo3 Mo1 . . 58.18(3) Cl5 Mo3 Mo1 . . 117.576(17) Mo2 Mo3 Mo1 3_775 . 60.21(2) Cl3 Mo3 Mo2 . . 136.56(2) Cl4 Mo3 Mo2 3_775 . 118.04(2) Cl6 Mo3 Mo2 . . 117.865(19) Cl7 Mo3 Mo2 . . 58.01(2) Cl5 Mo3 Mo2 . . 57.785(18) Mo2 Mo3 Mo2 3_775 . 89.853(15) Mo1 Mo3 Mo2 . . 59.808(16) Cl3 Mo3 Mo1 . 3_775 135.07(2) Cl4 Mo3 Mo1 3_775 3_775 58.001(17) Cl6 Mo3 Mo1 . 3_775 118.13(2) Cl7 Mo3 Mo1 . 3_775 118.052(17) Cl5 Mo3 Mo1 . 3_775 57.84(2) Mo2 Mo3 Mo1 3_775 3_775 59.883(12) Mo1 Mo3 Mo1 . 3_775 90.106(16) Mo2 Mo3 Mo1 . 3_775 60.054(15) Mo1 Cl4 Mo3 . 3_775 63.92(2) Mo1 Cl4 Mo2 . . 63.62(2) Mo3 Cl4 Mo2 3_775 . 63.55(3) Mo2 Cl5 Mo1 . 3_775 64.10(2) Mo2 Cl5 Mo3 . . 63.811(16) Mo1 Cl5 Mo3 3_775 . 63.834(16) Mo1 Cl6 Mo2 . 3_775 63.826(19) Mo1 Cl6 Mo3 . . 63.709(19) Mo2 Cl6 Mo3 3_775 . 63.43(2) Mo2 Cl7 Mo3 . . 63.744(17) Mo2 Cl7 Mo1 . . 63.534(17) Mo3 Cl7 Mo1 . . 63.64(2) C19 O1 C3 . . 120.45(16) C9 O2 C7 . . 120.23(17) C15 O3 C13 . . 120.38(17) C8 C1 C14 . . 119.9(2) C8 C1 C2 . . 120.2(2) C14 C1 C2 . . 119.9(2) C7 C2 C1 . . 119.4(2) C7 C2 C3 . . 120.8(2) C1 C2 C3 . . 119.7(2) C4 C3 O1 . . 120.01(19) C4 C3 C2 . . 120.0(2) O1 C3 C2 . . 120.01(19) C3 C4 C5 . . 119.2(2) C4 C5 C6 . . 121.1(2) C4 C5 C20 . . 121.44(19) C6 C5 C20 . . 117.42(19) C7 C6 C5 . . 118.8(2) O2 C7 C6 . . 119.49(19) O2 C7 C2 . . 120.41(19) C6 C7 C2 . . 120.1(2) C1 C8 C9 . . 119.8(2) C1 C8 C13 . . 120.2(2) C9 C8 C13 . . 120.04(19) C10 C9 O2 . . 120.18(19) C10 C9 C8 . . 119.8(2) O2 C9 C8 . . 119.97(19) C9 C10 C11 . . 119.6(2) C10 C11 C12 . . 121.06(19) C10 C11 C24 . . 120.83(19) C12 C11 C24 . . 118.01(19) C13 C12 C11 . . 118.9(2) C12 C13 O3 . . 119.94(19) C12 C13 C8 . . 120.53(19) O3 C13 C8 . . 119.53(19) C1 C14 C15 . . 119.54(19) C1 C14 C19 . . 119.8(2) C15 C14 C19 . . 120.62(19) C16 C15 O3 . . 119.88(19) C16 C15 C14 . . 119.67(19) O3 C15 C14 . . 120.44(18) C15 C16 C17 . . 119.8(2) C16 C17 C18 . . 120.6(2) C16 C17 C28 . . 118.79(19) C18 C17 C28 . . 120.54(19) C19 C18 C17 . . 119.5(2) C18 C19 O1 . . 120.16(19) C18 C19 C14 . . 119.8(2) O1 C19 C14 . . 120.00(19) C5 C20 C22 . . 112.26(18) C5 C20 C21 . . 108.31(18) C22 C20 C21 . . 109.96(19) C5 C20 C23 . . 108.90(19) C22 C20 C23 . . 108.21(19) C21 C20 C23 . . 109.15(19) C11 C24 C25 . . 112.46(19) C11 C24 C26 . . 110.38(18) C25 C24 C26 . . 108.61(19) C11 C24 C27 . . 106.19(19) C25 C24 C27 . . 109.1(2) C26 C24 C27 . . 110.1(2) C31 C28 C17 . . 110.95(18) C31 C28 C30 . . 108.21(19) C17 C28 C30 . . 107.06(18) C31 C28 C29 . . 108.57(19) C17 C28 C29 . . 111.69(18) C30 C28 C29 . . 110.29(19) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Mo1 Cl1 . 2.4404(7) Mo1 Cl5 3_775 2.4667(10) Mo1 Cl4 . 2.4692(7) Mo1 Cl6 . 2.4729(7) Mo1 Cl7 . 2.4770(10) Mo1 Mo2 . 2.6047(5) Mo1 Mo3 . 2.6121(6) Mo1 Mo3 3_775 2.6152(5) Mo1 Mo2 3_775 2.6159(6) Mo2 Cl2 . 2.4207(7) Mo2 Cl5 . 2.4631(8) Mo2 Cl7 . 2.4705(7) Mo2 Cl4 . 2.4724(7) Mo2 Cl6 3_775 2.4756(7) Mo2 Mo3 3_775 2.6033(9) Mo2 Mo3 . 2.6124(5) Mo2 Mo1 3_775 2.6159(6) Mo3 Cl3 . 2.4358(7) Mo3 Cl4 3_775 2.4712(7) Mo3 Cl6 . 2.4765(7) Mo3 Cl7 . 2.4770(8) Mo3 Cl5 . 2.4797(7) Mo3 Mo2 3_775 2.6032(9) Mo3 Mo1 3_775 2.6152(5) Cl4 Mo3 3_775 2.4713(7) Cl5 Mo1 3_775 2.4668(10) Cl6 Mo2 3_775 2.4755(7) O1 C19 . 1.382(3) O1 C3 . 1.385(3) O2 C9 . 1.380(3) O2 C7 . 1.382(3) O3 C15 . 1.377(2) O3 C13 . 1.384(2) C1 C8 . 1.385(3) C1 C14 . 1.394(3) C1 C2 . 1.395(3) C2 C7 . 1.396(3) C2 C3 . 1.405(3) C3 C4 . 1.376(3) C4 C5 . 1.407(3) C5 C6 . 1.413(3) C5 C20 . 1.532(3) C6 C7 . 1.383(3) C8 C9 . 1.405(3) C8 C13 . 1.408(3) C9 C10 . 1.375(3) C10 C11 . 1.400(3) C11 C12 . 1.411(3) C11 C24 . 1.529(3) C12 C13 . 1.369(3) C14 C15 . 1.402(3) C14 C19 . 1.405(3) C15 C16 . 1.376(3) C16 C17 . 1.405(3) C17 C18 . 1.407(3) C17 C28 . 1.532(3) C18 C19 . 1.377(3) C20 C22 . 1.535(3) C20 C21 . 1.541(3) C20 C23 . 1.542(3) C24 C25 . 1.532(3) C24 C26 . 1.536(3) C24 C27 . 1.535(3) C28 C31 . 1.530(3) C28 C30 . 1.540(3) C28 C29 . 1.539(3)