#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003214.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_2003214 _journal_name_full 'Acta Crystallographica' _journal_volume C51 _journal_year 1995 _journal_page_first 190 _journal_page_last 193 _publ_section_title ; Bis(hexadecylpyridinium) Bis(3,6-dichloro-4,5- dihydroxy-3,5-cyclohexadiene-1,2-dionato-\k^2^O^4^,O^5^)]beryllium ; loop_ _publ_author_name 'Hans Burzlaff' 'Joachim Lange' 'Roland Spengler' 'Miltiadis I. Karayannis' 'Panos G. Veltsistas' _chemical_formula_sum 'C54 H76 Be1 Cl4 N2 O8' _chemical_formula_structural ' 2C21 H38 N [Be(C6 Cl2 O4)2]' _chemical_formula_weight 1032.03 loop_ _symmetry_equiv_pos_as_xyz +x, +y, +z -x, -y, -z _symmetry_space_group_name_H-M 'P -1' _cell_length_a 10.3254(3) _cell_length_b 11.2915(2) _cell_length_c 25.0237(5) _cell_angle_alpha 85.981(3) _cell_angle_beta 80.177(3) _cell_angle_gamma 78.517(3) _cell_volume 2815.2(4) _cell_formula_units_Z 2 _exptl_crystal_density_diffrn 1.217 _diffrn_radiation_type 'Mo K\a1' _diffrn_radiation_wavelength 0.7107 _cell_measurement_reflns_used 32 _cell_measurement_theta_min 7.4 _cell_measurement_theta_max 10.6 _exptl_absorpt_coefficient_mu 0.2592 _cell_measurement_temperature 293 _exptl_crystal_description 'parallelepiped' _exptl_crystal_size_max .31 _exptl_crystal_size_mid .18 _exptl_crystal_size_min .13 _exptl_crystal_colour 'red' _diffrn_measurement_device 'rebuilt Philips PW1100 diffractometer (Gomm, 199 _diffrn_measurement_method \q/2\q _exptl_absorpt_correction_type 'gaussian integration (Busing & Levy, 1957)' _exptl_absorpt_correction_T_min 0.940 _exptl_absorpt_correction_T_max 0.971 _diffrn_reflns_number 18804 _reflns_number_total 9401 _reflns_number_observed 4863 _reflns_observed_criterion F>1.4\s(F) _diffrn_reflns_av_r_equivalents 0.0431 _diffrn_reflns_theta_max 25.0 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_decay_% 2.5 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.068 _refine_ls_wR_factor_obs 0.032 _refine_ls_goodness_of_fit_obs 1.44 _refine_ls_number_reflns 4863 _refine_ls_number_parameters 851 _refine_ls_hydrogen_treatment 'refall' _refine_ls_weighting_scheme ' w = 1/[\s^2^(F~o~)] ' _refine_ls_shift/esd_max 0.01 _refine_diff_density_max .31 _refine_diff_density_min -.47 _refine_ls_extinction_method 'none' loop_ _atom_type_symbol _atom_type_scat_source Cl International_Tables_Vol_IV_Table_2.2B O International_Tables_Vol_IV_Table_2.2B N International_Tables_Vol_IV_Table_2.2B C International_Tables_Vol_IV_Table_2.2B Be International_Tables_Vol_IV_Table_2.2B H International_Tables_Vol_IV_Table_2.2B loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_u_iso_or_equiv Cl(1) .0036(1) .3956(1) .24004(5) .0834(6) Cl(2) .3306(1) .2613(1) .00644(5) .0800(6) Cl(3) .3115(1) .94273(9) .07040(5) .0851(6) Cl(4) .7218(1) .6049(1) .20389(5) .0773(6) O(1) .3690(2) .4393(2) .0862(1) .057(1) O(2) .2339(2) .4985(2) .1746(1) .058(1) O(3) -.0273(3) .2057(2) .1677(1) .084(2) O(4) .0815(3) .1788(2) .0631(1) .081(2) O(5) .4895(2) .5450(2) .1570(1) .056(1) O(6) .3237(2) .6782(2) .1089(1) .059(1) O(7) .5513(3) .9994(2) .1060(1) .093(2) O(8) .7080(3) .8667(2) .1713(1) .075(1) N(1) .3050(3) .7347(3) .8856(1) .051(2) N(2) -.0145(3) .1408(4) .8452(2) .059(2) C(1) .2729(4) .3792(3) .0994(2) .049(2) C(2) .1921(4) .4146(3) .1537(2) .050(2) C(3) .0896(4) .3592(4) .1763(2) .056(2) C(4) .0562(4) .2668(4) .1490(2) .060(2) C(5) .1276(4) .2428(3) .0893(2) .058(2) C(6) .2407(4) .2970(3) .0696(2) .055(2) C(7) .5145(4) .6532(4) .1492(2) .048(2) C(8) .4143(4) .7338(4) .1195(2) .050(2) C(9) .4241(4) .8502(3) .1058(2) .055(2) C(10) .5307(4) .8987(4) .1194(2) .058(2) C(11) .6261(4) .8193(4) .1551(2) .056(2) C(12) .6134(4) .6959(4) .1661(2) .055(2) C(13) .3281(5) .7658(4) .9330(2) .071(2) C(14) .3033(5) .6955(5) .9789(2) .084(3) C(15) .2578(5) .5918(5) .9756(2) .088(3) C(16) .2363(5) .5604(4) .9271(2) .077(3) C(17) .2606(4) .6329(4) .8815(2) .063(2) C(18) .3372(4) .8104(4) .8356(2) .056(2) C(19) .4841(4) .7750(4) .8115(2) .063(2) C(20) .5178(4) .8648(4) .7651(2) .064(2) C(21) .6641(5) .8372(4) .7403(2) .076(2) C(22) .7025(5) .9331(4) .6982(2) .073(2) C(23) .8443(5) .9039(4) .6688(2) .073(2) C(24) .8825(5) 1.0045(4) .6298(2) .075(2) C(25) 1.0229(5) .9777(4) .5982(2) .073(2) C(26) 1.0599(5) 1.0809(4) .5610(2) .075(2) C(27) 1.1997(5) 1.0556(4) .5289(2) .072(2) C(28) 1.2339(5) 1.1609(4) .4919(2) .071(2) C(29) 1.3749(5) 1.1369(4) .4599(2) .072(2) C(30) 1.4068(5) 1.2416(4) .4228(2) .076(2) C(31) 1.5469(5) 1.2203(4) .3906(2) .079(3) C(32) 1.5747(6) 1.3257(5) .3533(2) .099(3) C(33) 1.7127(7) 1.3084(6) .3202(3) .128(4) C(34) -.0248(4) .2590(5) .8494(3) .073(3) C(35) .0057(6) .2992(6) .8937(3) .095(3) C(36) .0466(6) .2244(8) .9343(3) .098(4) C(37) .0557(5) .1021(7) .9314(3) .096(3) C(38) .0235(5) .0597(4) .8842(3) .074(2) C(39) -.0467(6) .0955(5) .7944(3) .091(3) C(40) .0803(7) .0589(5) .7539(2) .094(3) C(41) .1334(5) .1636(5) .7228(2) .080(3) C(42) .2660(6) .1290(5) .6860(2) .090(3) C(43) .3146(6) .2315(5) .6524(2) .092(3) C(44) .4485(7) .2028(6) .6169(2) .098(3) C(45) .4947(6) .3034(5) .5815(3) .097(3) C(46) .6292(7) .2794(6) .5485(2) .101(3) C(47) .6720(6) .3812(5) .5138(3) .100(3) C(48) .8088(7) .3588(5) .4819(3) .106(4) C(49) .8525(7) .4597(6) .4470(3) .106(4) C(50) .9899(7) .4395(6) .4156(3) .106(4) C(51) 1.0291(7) .5414(5) .3803(3) .107(4) C(52) 1.1679(7) .5232(6) .3509(3) .103(3) C(53) 1.2053(8) .6215(7) .3142(4) .154(6) C(54) 1.338(1) .6216(7) .2893(4) .147(6) Be(1) .3566(6) .5384(5) .1325(2) .058(3) H(1) .366(3) .840(2) .933(1) .0898(2) H(2) .318(3) .717(2) 1.015(1) .0898(2) H(3) .239(3) .540(2) 1.009(1) .0898(2) H(4) .204(3) .489(2) .921(1) .0898(2) H(5) .248(3) .616(2) .845(1) .0898(2) H(6) .314(2) .901(2) .847(1) .0898(2) H(7) .276(3) .801(2) .809(1) .0898(2) H(8) .538(2) .783(2) .843(1) .0898(2) H(9) .507(3) .692(2) .798(1) .0898(2) H(10) .492(3) .945(2) .779(1) .0898(2) H(11) .457(3) .857(2) .737(1) .0898(2) H(12) .719(3) .832(3) .771(1) .0898(2) H(13) .682(3) .756(2) .725(1) .0898(2) H(14) .689(3) 1.018(2) .717(1) .0898(2) H(15) .640(3) .947(3) .675(1) .0898(2) H(16) .904(3) .880(3) .694(1) .0898(2) H(17) .861(3) .827(2) .649(1) .0898(2) H(18) .870(3) 1.080(2) .648(1) .0898(2) H(19) .812(3) 1.026(2) .604(1) .0898(2) H(20) 1.084(3) .956(3) .625(1) .0898(2) H(21) 1.031(3) .903(2) .576(1) .0898(2) H(22) 1.050(3) 1.149(2) .581(1) .0898(2) H(23) .989(2) 1.108(3) .536(1) .0898(2) H(24) 1.269(2) 1.023(2) .556(1) .0898(2) H(25) 1.200(3) .986(2) .505(1) .0898(2) H(26) 1.223(3) 1.232(2) .516(1) .0898(2) H(27) 1.166(3) 1.198(3) .469(1) .0898(2) H(28) 1.441(3) 1.108(3) .485(1) .0898(2) H(29) 1.372(3) 1.070(3) .438(1) .0898(2) H(30) 1.390(3) 1.317(2) .444(1) .0898(2) H(31) 1.340(3) 1.271(3) .400(1) .0898(2) H(32) 1.628(3) 1.194(2) .415(1) .0898(2) H(33) 1.565(3) 1.142(2) .369(1) .0898(2) H(34) 1.567(3) 1.401(2) .378(1) .0898(2) H(35) 1.507(3) 1.348(3) .324(1) .0898(2) H(36) 1.775(3) 1.279(3) .345(1) .0898(2) H(37) 1.747(3) 1.218(3) .306(1) .0898(2) H(38) 1.715(3) 1.380(3) .298(1) .0898(2) H(39) -.066(3) .318(2) .814(1) .0898(2) H(40) .002(3) .381(3) .894(1) .0898(2) H(41) .053(3) .261(3) .967(1) .0898(2) H(42) .084(3) .032(2) .946(1) .0898(2) H(43) .027(3) -.019(2) .878(1) .0898(2) H(44) -.117(3) .178(2) .786(1) .0898(2) H(45) -.075(3) .026(3) .806(1) .0898(2) H(46) .078(3) .007(2) .729(1) .0898(2) H(47) .149(3) .014(3) .770(1) .0898(2) H(48) .064(3) .197(2) .698(1) .0898(2) H(49) .135(3) .226(2) .749(1) .0898(2) H(50) .264(3) .068(3) .664(1) .0898(2) H(51) .338(3) .102(2) .713(1) .0898(2) H(52) .246(3) .262(3) .626(1) .0898(2) H(53) .294(3) .308(2) .675(1) .0898(2) H(54) .452(3) .129(2) .597(1) .0898(2) H(55) .509(3) .186(3) .642(1) .0898(2) H(56) .415(3) .336(3) .562(1) .0898(2) H(57) .472(3) .378(2) .603(1) .0898(2) H(58) .639(3) .207(2) .527(1) .0898(2) H(59) .691(3) .270(3) .578(1) .0898(2) H(60) .602(3) .401(3) .485(1) .0898(2) H(61) .664(3) .449(2) .539(1) .0898(2) H(62) .825(3) .280(2) .465(1) .0898(2) H(63) .870(3) .340(3) .513(1) .0898(2) H(64) .793(3) .469(3) .421(1) .0898(2) H(65) .839(3) .535(2) .469(1) .0898(2) H(66) .997(3) .372(3) .396(1) .0898(2) H(67) 1.052(3) .424(3) .445(1) .0898(2) H(68) .969(3) .538(3) .346(1) .0898(2) H(69) 1.015(3) .615(3) .404(1) .0898(2) H(70) 1.190(3) .439(2) .327(1) .0898(2) H(71) 1.235(3) .507(3) .382(1) .0898(2) H(72) 1.136(4) .668(4) .317(2) .0898(2) H(73) 1.194(4) .696(3) .338(1) .0898(2) H(74) 1.369(3) .534(3) .270(1) .0898(2) H(75) 1.393(3) .577(3) .309(1) .0898(2) H(76) 1.344(4) .682(3) .265(1) .0898(2) loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Cl(1) .0687(8) -.0384(6) .0216(9) .1056(7) .0069(8) .095(1) Cl(2) .097(1) -.0495(6) .011(1) .0920(6) -.0090(7) .075(1) Cl(3) .0832(9) -.0324(5) -.023(1) .0678(6) .0263(7) .117(2) Cl(4) .0750(9) -.0332(5) -.024(1) .0791(6) .0075(7) .092(1) O(1) .055(2) -.038(1) .009(2) .067(1) -.004(2) .073(3) O(2) .059(2) -.038(1) .006(2) .069(1) -.002(2) .067(3) O(3) .065(2) -.055(1) .002(2) .096(2) .012(2) .123(4) O(4) .089(2) -.059(1) -.026(3) .088(2) .011(2) .100(4) O(5) .054(2) -.032(1) -.006(2) .055(1) .008(2) .077(3) O(6) .050(2) -.032(1) -.010(2) .065(1) .009(2) .079(3) O(7) .126(3) -.078(2) -.021(3) .084(1) .017(2) .111(4) O(8) .062(2) -.041(1) -.009(2) .081(2) -.011(2) .104(4) N(1) .052(2) -.023(1) .004(2) .056(2) .006(2) .056(4) N(2) .049(2) -.030(2) .001(3) .072(2) .005(3) .072(4) C(1) .049(3) -.022(2) -.002(3) .049(2) .014(2) .062(5) C(2) .046(3) -.022(2) -.006(3) .055(2) .012(2) .060(5) C(3) .046(3) -.026(2) .001(3) .065(2) .017(3) .071(5) C(4) .045(3) -.026(2) -.010(3) .063(2) .021(3) .088(6) C(5) .059(3) -.026(2) -.014(4) .045(2) .018(2) .083(6) C(6) .056(3) -.027(2) -.001(3) .055(2) .003(3) .068(5) C(7) .043(3) -.024(2) .006(3) .055(2) -.001(2) .060(4) C(8) .043(3) -.024(2) .000(3) .058(2) .001(2) .061(4) C(9) .050(3) -.023(2) -.002(3) .049(2) .004(2) .077(5) C(10) .069(3) -.035(2) .009(3) .055(2) -.005(3) .067(5) C(11) .044(3) -.023(2) .009(3) .067(2) -.012(3) .070(5) C(12) .051(3) -.027(2) -.001(3) .061(2) .000(2) .067(5) C(13) .095(4) -.061(2) .000(4) .094(3) .003(3) .059(5) C(14) .115(4) -.062(3) .009(4) .116(3) .005(4) .056(6) C(15) .100(4) -.033(3) .027(5) .091(3) .017(4) .084(7) C(16) .084(4) -.036(2) .017(5) .058(2) .005(4) .104(7) C(17) .068(3) -.032(2) .005(4) .058(2) .002(3) .079(6) C(18) .058(3) -.029(2) .003(3) .070(2) .020(3) .055(5) C(19) .061(3) -.022(2) .016(3) .068(2) .014(3) .068(5) C(20) .059(3) -.024(2) .016(3) .074(2) .014(3) .070(5) C(21) .074(4) -.030(3) .023(4) .081(2) .024(3) .086(6) C(22) .065(4) -.027(3) .019(4) .084(3) .009(3) .082(6) C(23) .071(4) -.032(2) .019(4) .083(3) .008(3) .080(6) C(24) .078(4) -.034(3) .020(4) .076(2) .009(3) .088(6) C(25) .072(4) -.036(3) .024(4) .089(3) .005(3) .078(6) C(26) .084(4) -.039(3) .020(4) .083(3) .008(3) .077(6) C(27) .069(4) -.032(2) .019(4) .086(3) .005(3) .078(6) C(28) .077(4) -.034(2) .025(4) .074(2) .006(3) .078(6) C(29) .075(4) -.032(2) .014(4) .082(3) .012(3) .075(6) C(30) .076(4) -.034(2) .025(4) .077(3) .006(3) .092(6) C(31) .072(4) -.031(3) .024(4) .091(3) .005(3) .088(6) C(32) .089(5) -.049(3) .029(5) .121(4) .015(4) .112(8) C(33) .116(6) -.057(4) .039(6) .150(4) .028(5) .15(1) C(34) .055(3) -.022(2) .002(4) .079(4) -.008(4) .095(7) C(35) .074(4) -.050(4) .017(5) .122(4) -.029(7) .120(9) C(36) .076(4) -.049(4) .006(5) .168(6) -.023(6) .079(8) C(37) .067(4) -.031(4) .005(5) .144(5) .036(5) .092(8) C(38) .060(3) -.034(3) .007(4) .086(3) .019(5) .094(7) C(39) .087(5) -.058(3) -.017(5) .125(4) -.001(5) .093(7) C(40) .136(6) -.057(3) -.003(6) .098(3) -.008(4) .072(7) C(41) .078(4) -.029(3) -.008(4) .092(3) .005(3) .080(7) C(42) .127(5) -.042(3) .001(5) .097(3) .002(4) .061(7) C(43) .093(5) -.017(3) .008(5) .084(3) -.010(4) .100(7) C(44) .126(6) -.032(4) .011(5) .099(3) .002(4) .077(7) C(45) .097(5) -.015(3) .006(5) .074(3) -.007(4) .119(8) C(46) .117(6) -.030(4) .015(5) .104(3) .006(4) .090(8) C(47) .101(5) -.032(3) .012(5) .102(4) -.007(4) .108(8) C(48) .126(6) -.034(4) .018(6) .100(3) .009(5) .101(8) C(49) .096(6) -.033(4) .004(6) .109(4) -.014(5) .13(1) C(50) .116(6) -.029(4) .006(6) .102(4) .014(5) .107(9) C(51) .105(5) -.039(4) .019(6) .110(4) -.021(5) .122(9) C(52) .125(6) -.046(4) .001(6) .111(3) .009(4) .093(8) C(53) .112(8) -.028(4) .062(9) .123(6) -.020(7) .23(2) C(54) .178(9) -.055(6) .016(9) .159(6) .031(5) .12(1) Be(1) .051(4) -.026(2) -.002(4) .059(3) .010(4) .078(7)