#------------------------------------------------------------------------------ #$Date: 2011-09-17 23:27:16 +0300 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2001847.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_2001847 loop_ _publ_author_name 'Yamada, K.' 'Hori, K.' 'Fukuda, Y.' _publ_section_title ; Structure of \m-carbonato-1\k^2^O^1^,O^2^:2\k^2^O^1^,O^3^-bis[(acetylacetonato)(N,N,N',N'-tetramethylethylenediamine)nickel(II)] (acetylacetonato)aqua(methanol)(N,N,N',N'-tetramethylethylenediamine)nickel(II) tetraphenylborate ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 445 _journal_page_last 448 _journal_volume 49 _journal_year 1993 _chemical_formula_sum 'C59 H95 B N6 Ni3 O11' _[local]_cod_chemical_formula_sum_orig 'C59 H95 B1 N6 Ni3 O11' _chemical_formula_weight 1251.32 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 97.41(6) _cell_angle_beta 95.29(6) _cell_angle_gamma 117.83(3) _cell_formula_units_Z 2 _cell_length_a 16.965(9) _cell_length_b 18.847(8) _cell_length_c 12.108(7) _cell_volume 3344(3) _diffrn_radiation_type Mo _diffrn_radiation_wavelength 0.71069 _exptl_absorpt_coefficient_mu .894 _exptl_crystal_density_diffrn 1.243 _exptl_crystal_F_000 1336 _[local]_cod_data_source_file as1009.cif _[local]_cod_data_source_block as1009_structure_1_of_1 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z Ni(1) .61383(2) .84231(2) .56929(3) Ni(2) .64839(2) .74936(2) .85928(3) O(1) .63500(10) .80150(10) .7185(2) O(2) .53920(10) .77630(10) .8383(2) O(3) .52530(10) .83130(10) .6878(2) C(1) .5650(2) .8035(2) .7491(3) O(11) .5338(2) .72290(10) .4993(2) O(12) .5603(2) .8733(2) .4418(2) O(21) .72990(10) .86300(10) .9530(2) O(22) .75600(10) .73690(10) .8321(2) N(11) .7017(2) .9703(2) .6402(2) N(12) .7267(2) .8498(2) .4984(2) N(21) .5652(2) .6243(2) .7692(2) N(22) .6253(2) .6963(2) 1.0054(2) C(11) .4700(3) .6937(2) .4158(3) C(12) .4104(4) .6044(3) .3928(5) C(13) .4521(3) .7409(3) .3479(4) C(14) .4966(2) .8253(3) .3611(3) C(15) .4678(4) .8648(4) .2804(5) C(16) .7386(5) .9887(3) .7581(4) C(17) .6587(4) 1.0193(3) .6278(7) C(18) .7696(3) .9932(3) .5670(6) C(19) .8004(3) .9349(3) .5403(4) C(20) .7076(3) .8340(4) .3742(4) C(21) .7526(3) .7918(3) .5367(4) C(31) .8133(2) .9057(2) .9476(3) C(32) .8592(3) .9935(3) 1.0092(4) C(33) .8647(2) .8767(2) .8934(3) C(34) .8358(2) .7957(2) .8444(3) C(35) .9033(3) .7735(3) .7988(4) C(36) .4682(3) .5998(2) .7367(4) C(37) .5982(3) .6078(2) .6653(4) C(38) .5780(3) .5778(2) .8517(4) C(39) .5638(3) .6075(2) .9661(4) C(40) .7115(3) .7105(3) 1.0693(4) C(41) .5828(3) .7322(3) 1.0778(3) Ni(3) .71547(2) .212301(2) .19839(3) O(W) .60890(10) .22330(10) .1031(2) O(Me) .6277(2) .1689(2) .3140(2) C(Me) .6275(3) .1248(3) .3982(4) O(31) .79900(10) .1804(2) .2783(2) O(32) .6504(2) .10170(10) .0950(2) N(31) .7806(2) .3319(2) .2971(3) N(32) .8064(2) .2665(2) .0840(3) C(51) .7907(2) .1098(2) .2634(3) C(52) .8635(3) .1035(3) .3390(4) C(53) .7238(3) .0418(2) .1881(4) C(54) .6592(3) .0403(2) .1088(4) C(55) .5927(3) -.0393(3) .0284(4) C(56) .8183(4) .3369(3) .4134(4) C(57) .7188(3) .3667(3) .3045(4) C(58) .8553(4) .3806(3) .2407(6) C(59) .8497(6) .3533(4) .1333(7) C(60) .7577(4) .2498(5) -.0320(5) C(61) .8676(4) .2342(4) .0711(6) B .0751(2) .3366(2) .7431(3) C(71) .0580(2) .2412(2) .7267(3) C(72) .0615(3) .2027(2) .8140(4) C(73) .0458(3) .1208(3) .7980(4) C(74) .0269(3) .0773(2) .6904(5) C(75) .0222(3) .1139(2) .6003(4) C(76) .0380(2) .1932(2) .6189(3) C(77) -.0222(2) .3362(2) .7453(3) C(78) -.1052(2) .2710(2) .6901(3) C(79) -.1843(3) .2771(3) .6828(4) C(80) -.1828(3) .3478(4) .72621(5) C(81) -.1024(3) .4125(3) .7872(6) C(82) -.0242(3) .4064(2) .7944(5) C(83) .1161(2) .3741(2) .6330(3) C(84) .0745(3) .4006(2) .5578(3) C(85) .1106(4) .4292(3) .4619(4) C(86) .1891(4) .4305(3) .4407(4) C(87) .2336(3) .4064(3) .5141(4) C(88) .1971(3) .3769(2) .6078(4) C(89) .1430(2) .3939(2) .8624(3) C(90) .2293(2) .4606(2) .8681(4) C(91) .2821(3) .5102(3) .9720(5) C(92) .2518(4) .4941(3) 1.0707(4) C(93) .1678(4) .4291(3) 1.0687(4) C(94) .1156(3) .3811(3) .9663(4) H(121) .369(3) .572(3) .319(4) H(122) .381(6) .583(5) .456(7) H(123) .466(6) .596(5) .393(7) H(131) .417(3) .722(3) .287(4) H(151) .417(5) .825(4) .219(6) H(152) .523(6) .896(5) .247(7) H(153) .451(6) .905(5) .320(7) H(161) .768(5) .955(5) .769(7) H(162) .688(3) .973(2) .804(3) H(163) .784(3) 1.048(3) .787(4) H(171) .629(3) 1.013(3) .550(4) H(172) .703(3) 1.078(3) .659(4) H(173) .609(6) 1.001(5) .677(7) H(181) .728(6) 1.001(5) .509(7) H(182) .818(3) 1.048(3) .607(4) H(191) .828(5) .939(5) .619(7) H(192) .849(3) .954(2) .493(3) H(201) .691(5) .872(5) .340(7) H(202) .653(6) .777(5) .356(7) H(203) .758(5) .832(4) .342(6) H(211) .768(6) .799(5) .619(8) H(212) .804(5) .795(4) .500(6) H(213) .698(6) .736(6) .506(8) H(321) .919(6) 1.033(5) .992(7) H(322) .866(6) .989(5) 1.091(7) H(323) .814(6) 1.013(5) .995(8) H(331) .919(2) .910(2) .898(3) H(351) .962(3) .823(3) .795(4) H(352) .878(3) .737(3) .723(4) H(353) .915(6) .744(5) .856(7) H(361) .442(5) .604(4) .806(6) H(362) .437(2) .541(2) .696(3) H(363) .459(3) .634(3) .686(4) H(371) .663(4) .622(3) .682(5) H(372) .591(2) .642(2) .612(3) H(373) .561(4) .549(4) .630(5) H(381) .534(4) .518(3) .827(5) H(382) .641(3) .586(3) .853(4) H(391) .573(3) .574(3) 1.018(4) H(392) .499(4) .594(3) .957(5) H(401) .743(3) .690(2) 1.019(4) H(402) .700(3) .681(2) 1.135(3) H(403 .749(3) .770(3) 1.098(4) H(411) .525(2) .727(2) 1.042(3) H(412) .629(3) .792(2) 1.104(4) H(413) .574(3) .704(3) 1.144(4) H(W1) .576(4) .167(4) .070(5) H(W2) .566(3) .226(3) .1361(4) H(MO) .593(4) .174(3) .317(5) H(Me1) .691(6) .132(5) .403(7) H(Me2) .616(6) .138(5) .475(8) H(Me3) .583(6) .066(5) .362(7) H(521) .923(6) .104(5) .345(7) H(522) .874(5) .160(5) .333(7) H(523) .838(5) .090(4) .411(6) H(531) .749(5) .020(5) .182(7) H(551) .601(6) -.082(5) .058(7) H(552) .608(5) -.038(5) -.051(7) H(553) .528(5) -.052(5) .024(7) H(561) .776(6) .322(5) .471(7) H(562) .833(6) .291(5) .393(7) H(563) .875(5) .388(5) .447(6) H(571) .672(5) .336(5) .348(7) H(572) .734(6) .426(5) .317(7) H(573) .697(6) .343(5) .221(8) H(581) .818(6) .410(5) .244(7) H(582) .921(6) .423(5) .259(7) H(591) .892(5) .3301(5) .157(7) H(592) .883(6) .397(5) .090(7) H(601) .717(6) .208(5) -.103(7) H(602) .720(6) .258(5) .020(7) H(603) .798(6) .302(5) -.055(7) H(611) .851(4) .178(4) .029(6) H(612) .926(3) .275(3) .055(4) H(613) .874(5) .234(5) .155(8) H(72) .056(4) .236(3) .903(5) H(73) .048(3) .095(3) .861(4) H(74) .026(4) .011(4) .692(6) H(75) .031(4) .0761(3) .526(5) H(76) .040(3) .224(2) .555(3) H(78) -.115(3) .216(3) .661(4) H(79) -.2321(4) .240(3) .648(5) H(80) -.215(3) .356(2) .757(3) H(81) -.107(4) .462(4) .816(5) H(82) .035(5) .451(5) .837(7) H(84) .018(4) .386(4) .583(6) H(85) .086(4) .454(3) .409(5) H(86) .196(4) .462(3) .375(5) H(87) .306(6) .414(5) .481(7) H(88) .226(3) .350(2) .655(4) H(90) .270(3) .475(3) .795(4) H(91) .328(5) .543(4) .964(6) H(92) .286(4) .512(3) 1.149(5) H(93) .155(3) .414(2) 1.135(4) H(94) .061(4) .339(4) .973(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ni(1) O(1) 2.118(2) Ni(1) O(3) 2.131(3) Ni(1) O(11) 2.018(3) Ni(1) O(12) 2.004(3) Ni(1) N(11) 2.156(3) Ni(1) N(12) 2.123(3) Ni(2) O(1) 2.119(2) Ni(2) O(2) 2.139(2) Ni(2) O(21) 2.026(2) Ni(2) O(22) 1.997(3) Ni(2) N(21) 2.164(3) Ni(2) N(22) 2.122(3) O(1) C(1) 1.292(4) O(2) C(1) 1.281(4) O(3) C(1) 1.272(4) O(11) C(11) 1.263(5) O(12) C(14) 1.267(6) O(21) C(31) 1.273(5) O(22) C(34) 1.265(5) N(11) C(16) 1.433(9) N(11) C(17) 1.435(9) N(11) C(18) 1.456(8) N(12) C(19) 1.481(6) N(12) C(20) 1.470(7) N(12) C(21) 1.463(6) N(21) C(36) 1.484(5) N(21) C(37) 1.478(6) N(21) C(38) 1.475(6) N(22) C(39) 1.479(6) N(22) C(40) 1.478(6) N(22) C(41) 1.471(6) C(11) C(12) 1.473(8) C(11) C(13) 1.399(7) C(13) C(14) 1.384(7) C(14) C(15) 1.479(8) C(18) C(19) 1.437(9) C(31) C(32) 1.509(6) C(31) C(33) 1.395(6) C(33) C(34) 1.392(6) C(34) C(35) 1.514(7) C(38) C(39) 1.509(7) Ni(3) O(W) 2.160(3) Ni(3) O(Me) 2.094(3) Ni(3) O(31) 1.999(3) Ni(3) O(32) 2.014(3) Ni(3) N(31) 2.114(3) Ni(3) N(32) 2.151(4) O(Me) C(Me) 1.395(6) O(31) C(51) 1.257(5) O(32) C(54) 1.263(5) N(31) C(56) 1.465(8) N(31) C(57) 1.477(6) N(31) C(58) 1.466(8) N(32) C(59) 1.456(11) N(32) C(60) 1.477(11) N(32) C(61) 1.439(9) C(51) C(52) 1.529(7) C(51) C(53) 1.382(7) C(53) C(54) 1.376(7) C(54) C(55) 1.520(7) C(58) C(59) 1.313(12) B C(71) 1.663(6) B C(77) 1.649(6) B C(83) 1.649(6) B C(89) 1.645(6) C(71) C(72) 1.369(6) C(71) C(76) 1.402(5) C(72) C(73) 1.422(7) C(73) C(74) 1.369(8) C(74) C(75) 1.379(7) C(75) C(76) 1.373(6) C(77) C(78) 1.392(6) C(77) C(82) 1.396(7) C(78) C(79) 1.397(8) C(79) C(80) 1.355(9) C(80) C(81) 1.386(10) C(81) C(82) 1.380(9) C(83) C(84) 1.378(6) C(83) C(88) 1.414(6) C(84) C(85) 1.413(8) C(85) C(86) 1.370(9) C(86) C(87) 1.366(9) C(87) C(88) 1.397(7) C(89) C(90) 1.404(6) C(89) C(94) 1.393(6) C(90) C(91) 1.401(7) C(91) C(92) 1.359(9) C(92) C(93) 1.374(9) C(93) C(94) 1.378(9) loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O(1) Ni(1) O(3) 62.20(10) O(1) Ni(1) O(11) 86.00(10) O(1) Ni(1) O(12) 163.80(10) O(1) Ni(1) N(11) 94.90(10) O(1) Ni(1) N(12) 99.10(10) O(3) Ni(1) O(11) 89.50(10) O(3) Ni(1) O(12) 102.10(10) O(3) Ni(1) N(11) 92.20(10) O(3) Ni(1) N(12) 160.90(10) O(11) Ni(1) O(12) 90.10(10) O(11) Ni(1) N(11) 178.30(10) O(11) Ni(1) N(12) 93.70(10) O(12) Ni(1) N(11) 89.40(10) O(12) Ni(1) N(12) 96.80(10) N(11) Ni(1) N(12) 84.70(10) O(1) Ni(2) O(2) 62.40(10) O(1) Ni(2) O(21) 89.80(10) O(1) Ni(2) O(22) 99.20(10) O(1) Ni(2) N(21) 94.50(10) O(1) Ni(2) N(22) 163.20(10) O(2) Ni(2) O(21) 90.20(10) O(2) Ni(2) O(22) 161.50(10) O(2) Ni(2) N(21) 92.90(10) O(2) Ni(2) N(22) 100.90(10) O(21) Ni(2) O(22) 90.70(10) O(21) Ni(2) N(21) 175.50(10) O(21) Ni(2) N(22) 92.20(10) O(22) Ni(2) N(21) 87.40(10) O(22) Ni(2) N(22) 97.50(10) N(21) Ni(2) N(22) 84.00(10) Ni(1) O(1) Ni(2) 174.70(10) Ni(1) O(1) C(1) 89.9(2) Ni(2) O(1) C(1) 90.2(2) Ni(2) O(2) C(1) 89.5(2) Ni(1) O(3) C(1) 89.8(2) O(1) C(1) O(2) 117.9(3) O(1) C(1) O(3) 117.9(3) O(2) C(1) O(3) 124.2(3) O(W) Ni(3) O(Me) 86.50(10) O(W) Ni(3) O(31) 169.70(10) O(W) Ni(3) O(32) 80.00(10) O(W) Ni(3) N(31) 96.20(10) O(W) Ni(3) N(32) 91.80(10) O(Me) Ni(3) O(31) 89.70(10) O(Me) Ni(3) O(32) 90.80(10) O(Me) Ni(3) N(31) 91.10(10) O(Me) Ni(3) N(32) 175.30(10) O(31) Ni(3) O(32) 90.40(10) O(31) Ni(3) N(31) 93.50(10) O(31) Ni(3) N(32) 92.70(10) O(32) Ni(3) N(31) 175.70(10) O(32) Ni(3) N(32) 93.20(10) N(31) Ni(3) N(32) 84.70(10) _cod_database_code 2001847