#------------------------------------------------------------------------------ #$Date: 2022-10-03 15:40:12 +0100 (Mon, 03 Oct 2022) $ #$Revision: 278324 $ #$URL: svn://www.crystallography.net/cod/cif/2/10/09/2100973.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_2100973 loop_ _publ_author_name 'Maginn, S. J.' 'Harding, M. M.' 'Campbell, J. W.' _publ_section_title ; Structure determination of a complex pentamolybdodisulfate from synchrotron radiation Laue diffraction photographs: derivation and application of a wavelength-dependent absorption correction ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section B' _journal_page_first 520 _journal_page_last 524 _journal_paper_doi 10.1107/S0108768192011662 _journal_volume 49 _journal_year 1993 _chemical_formula_moiety '4(C8 H20 N1),C7 H5 N1,Mo5 O23 S2' _chemical_formula_sum 'C39 H85 Mo5 N5 O23 S2' _chemical_formula_weight 1530.8 _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _cell_angle_alpha 90 _cell_angle_beta 88.020(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.712(5) _cell_length_b 30.83(2) _cell_length_c 14.745(6) _cell_volume 5775(5) _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.6 _exptl_absorpt_coefficient_mu 4.289 _exptl_crystal_density_diffrn 1.76 _exptl_crystal_F_000 3100 _cod_data_source_file mu0303.cif _cod_data_source_block mu0303a _cod_original_cell_volume 5775.3 _cod_database_code 2100973 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 -x+1/2,y+1/2,-z+1/2 3 -x,-y,-z 4 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 Mo(1) -.01454(18) .13125(9) .65717(16) .0234(16) Mo(2) .36074(19) .09955(9) .84126(16) .0261(16) Mo(3) .24518(18) .11125(9) .61877(15) .0230(15) Mo(4) -.04840(19) .16154(10) .87916(17) .0312(17) Mo(5) .1785(2) .14366(10) .98981(16) .0329(17) S(1) .1042(5) .0700(2) .8167(5) .0243(18) S(2) .1933(5) .1895(3) .7747(5) .0244(18) O(3) .3345(13) .1006(6) .7168(11) .020(4) O(4) -.0831(16) .1330(7) .7755(14) .037(5) O(5) .0618(15) .1792(7) .9542(12) .031(5) O(6) .1097(14) .1329(6) .5882(12) .026(5) O(7) .0741(14) .1013(7) .8867(12) .027(5) O(8) .1108(14) .0948(6) .7299(12) .024(4) O(9) .0804(14) .1804(6) .7653(11) .023(4) O(10) .2303(16) .0617(7) .5803(14) .042(5) O(11) .457(2) .1392(10) .8386(18) .063(7) O(12) -.0727(15) .1738(7) .6103(13) .035(5) O(13) -.0716(15) .0897(7) .6095(13) .033(5) O(14) .0288(15) .0368(7) .8144(13) .035(5) O(15) .2122(16) .0531(7) .8324(13) .036(5) O(16) .2918(15) .1080(7) .9543(13) .033(5) O(17) .2350(16) .1596(7) .8431(14) .037(5) O(18) -.103(2) .2098(10) .8607(18) .065(7) O(19) .2069(17) .2341(8) .7975(15) .046(6) O(20) .4284(18) .0536(8) .8532(15) .050(6) O(21) .3252(18) .1321(8) .5436(15) .049(6) O(22) .2455(16) .1791(7) .6918(14) .041(6) O(23) .1253(19) .1154(9) 1.0718(16) .056(7) O(24) .2405(19) .1838(9) 1.0453(16) .054(6) O(25) -.133(2) .1403(9) .9549(17) .060(7) N(1) .593(2) .1956(10) .5868(18) .042(7) C(1) .487(4) .2068(16) .640(3) .070(12) C(2) .477(6) .253(2) .663(5) .112(19) C(3) .600(4) .2167(17) .500(3) .070(12) C(4) .515(4) .2083(18) .439(3) .078(13) C(5) .685(3) .2145(14) .637(3) .052(10) C(6) .687(4) .192(2) .737(4) .091(15) C(7) .593(4) .1497(17) .571(3) .072(12) C(8) .014(8) .347(4) 1.012(7) .15(3) N(2) .2766(19) -.0258(9) 1.0648(16) .034(6) C(11) .361(3) .0085(15) 1.090(3) .058(11) C(12) .323(3) .0418(16) 1.143(3) .064(12) C(13) .193(5) -.005(2) 1.004(4) .096(17) C(14) .111(4) -.0363(18) .972(3) .077(13) C(15) .332(4) -.0586(19) 1.022(4) .086(14) C(16) .368(5) -.047(3) .919(5) .112(19) C(17) .218(3) -.0392(14) 1.150(3) .059(11) C(18) .293(4) -.0620(18) 1.220(3) .080(14) N(3) .073(2) .2809(11) .557(2) .055(8) C(21) .132(3) .2380(12) .543(2) .039(8) C(22) .186(5) .234(2) .450(4) .099(16) C(23) .015(4) .2753(18) .641(3) .076(13) C(24) -.040(5) .320(2) .678(4) .103(17) C(25) .001(3) .2870(16) .475(3) .067(12) C(26) -.068(5) .259(2) .449(5) .106(19) C(27) .151(4) .316(2) .558(4) .086(15) C(28) .221(4) .3122(19) .636(4) .085(14) N(4) .004(2) .0807(9) 1.3382(17) .036(6) C(31) -.061(4) .1230(17) 1.395(3) .076(13) C(32) -.095(4) .149(2) 1.320(4) .088(15) C(33) .056(5) .061(3) 1.415(5) .12(2) C(34) .092(6) .103(3) 1.467(5) .15(2) C(35) -.071(4) .061(2) 1.289(4) .091(16) C(36) -.156(5) .034(2) 1.339(4) .107(18) C(37) .090(7) .100(4) 1.261(6) .15(3) C(38) .170(6) .129(3) 1.336(6) .13(2) C(41) .458(2) -.0531(8) .668(2) .067(11) C(42) .545(2) -.0662(8) .615(2) .089(15) C(43) .610(2) -.0355(8) .573(2) .099(17) C(44) .588(2) .0082(8) .584(2) .14(2) C(45) .501(2) .0213(8) .638(2) .067(11) C(46) .436(2) -.0094(8) .680(2) .060(11) C(47) .410(5) -.084(3) .700(4) .105(17) N(5) .357(6) -.107(3) .718(5) .14(2) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O(4) Mo(1) O(6) 148.2(9) O(12) Mo(1) O(13) 103.0(10) O(3) Mo(2) O(16) 140.7(8) O(11) Mo(2) O(20) 103.0(10) O(3) Mo(3) O(6) 143.7(8) O(10) Mo(3) O(21) 102.0(10) O(4) Mo(4) O(5) 146.1(9) O(18) Mo(4) O(25) 101.0(10) O(5) Mo(5) O(16) 148.0(8) O(23) Mo(5) O(24) 103.0(10) O(7) S(1) O(14) 110.0(10) O(8) S(1) O(14) 112.0(10) O(14) S(1) O(15) 112.0(10) O(9) S(2) O(19) 109.0(10) O(17) S(2) O(19) 113.0(10) O(19) S(2) O(22) 112.0(10) Mo(2) O(3) Mo(3) 152.0(10) Mo(1) O(4) Mo(4) 131.0(10) Mo(4) O(5) Mo(5) 126.0(10) Mo(1) O(6) Mo(3) 128.0(10) Mo(2) O(16) Mo(5) 131.0(10) C(11) N(2) C(13) 110(3) C(11) N(2) C(15) 105(3) C(11) N(2) C(17) 108(3) C(13) N(2) C(15) 113(4) C(13) N(2) C(17) 106(3) C(15) N(2) C(17) 115(3) N(2) C(11) C(12) 114(4) N(2) C(13) C(14) 113(4) N(2) C(15) C(16) 114(4) N(2) C(17) C(18) 112(3) C(42) C(41) C(47) 112(4) C(46) C(41) C(47) 128(4) C(41) C(47) N(5) 167(9) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Mo(1) O(4) 1.92(2) Mo(1) O(6) 1.85(2) Mo(1) O(8) 2.25(2) Mo(1) O(9) 2.52(2) Mo(1) O(12) 1.67(2) Mo(1) O(13) 1.64(2) Mo(2) O(3) 1.88(2) Mo(2) O(11) 1.73(3) MO(2) O(15) 2.38(2) Mo(2) O(16) 1.87(2) Mo(2) O(17) 2.45(2) Mo(2) O(20) 1.67(2) Mo(3) O(3) 1.90(2) Mo(3) O(6) 1.91(2) Mo(3) O(8) 2.38(2) Mo(3) O(10) 1.64(2) Mo(3) O(21) 1.61(2) Mo(3) O(22) 2.35(2) Mo(4) O(4) 1.83(2) Mo(4) O(5) 1.89(2) Mo(4) O(7) 2.43(2) Mo(4) O(9) 2.38(2) Mo(4) O(18) 1.67(3) Mo(4) O(25) 1.66(3) Mo(5) O(5) 1.93(2) Mo(5) O(7) 2.43(2) Mo(5) O(16) 1.87(2) Mo(5) O(17) 2.31(2) Mo(5) O(23) 1.62(3) Mo(5) O(24) 1.69(2) S(1) O(7) 1.46(2) S(1) O(8) 1.49(2) S(1) O(14) 1.40(2) S(1) O(15) 1.49(2) S(2) O(9) 1.47(2) S(2) O(17) 1.48(2) S(2) O(19) 1.43(2) S(2) O(22) 1.41(2) N(1) C(1) 1.58(5) N(1) C(3) 1.44(6) N(1) C(5) 1.52(5) N(1) C(7) 1.43(6) C(1) C(2) 1.47(9) C(3) C(4) 1.46(7) C(5) C(6) 1.64(7) C(7) C(8) 1.35(7) N(2) C(11) 1.56(5) N(2) C(13) 1.56(7) N(2) C(15) 1.37(6) N(2) C(17) 1.49(5) C(11) C(12) 1.37(6) C(13) C(14) 1.52(8) C(15) C(16) 1.61(9) C(17) C(18) 1.59(7) N(3) C(21) 1.53(5) N(3) C(23) 1.43(6) N(3) C(25) 1.56(6) N(3) C(27) 1.47(6) C(21) C(22) 1.52(7) C(23) C(24) 1.63(8) C(25) C(26) 1.31(8) C(27) C(28) 1.48(8) N(4) C(31) 1.74(7) N(4) C(33) 1.46(8) N(4) C(35) 1.36(6) N(4) C(37) 1.65(8) C(31) C(32) 1.44(8) C(33) C(34) 1.57(11) C(35) C(36) 1.52(9) C(37) C(38) 1.75(8) C(41) C(42) 1.39(4) C(41) C(46) 1.39(4) C(41) C(47) 1.20(8) C(42) C(43) 1.39(4) C(43) C(44) 1.39(4) C(44) C(45) 1.39(4) C(45) C(46) 1.39(4) C(47) N(5) 1.03(10)