#------------------------------------------------------------------------------ #$Date: 2011-09-17 23:27:16 +0300 (Sat, 17 Sep 2011) $ #$Revision: 26029 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/2013140.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_2013140 loop_ _publ_author_name 'Wikstad, Emma' 'Kritikos, Mikael' _publ_section_title ; (N~2~C~6~H~14~)~2~[VO(PO~3~OH)~5~B~2~O].H~2~O.H~3~PO~4~, a novel borophosphate cluster containing a single V centre and linked by hydrogen bonds into a three-dimensional framework ; _journal_name_full 'Acta Crystallographica, Section C' _journal_page_first m87 _journal_page_last m89 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '(N2 C6 H14)2 [V O (P O4 H)5 B2 O] , H2 O , H3 P O4' _chemical_formula_moiety '2C6 H14 N2 2+ , H5 B2 O22 P5 V 4- , H3 O4 P, H2 O' _chemical_formula_sum 'C12 H38 B2 N4 O27 P6 V' _chemical_formula_weight 928.84 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _cell_angle_alpha 90 _cell_angle_beta 94.113(12) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.4882(15) _cell_length_b 12.2569(13) _cell_length_c 19.6281(18) _cell_measurement_temperature 293(2) _cell_volume 3236.6(6) _diffrn_ambient_temperature 293(2) _exptl_crystal_density_diffrn 1.906 _[local]_cod_cif_authors_sg_H-M 'P 21/c' _[local]_cod_cif_authors_sg_Hall '-P 2ybc' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 2013140 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 V1 0.71828(3) 0.78670(3) 0.16028(2) 0.01453(10) Uani d . 1 . . V P1 0.74382(4) 0.96597(5) -0.08808(3) 0.01678(13) Uani d . 1 . . P P2 0.94315(4) 0.86147(5) 0.12056(3) 0.01900(14) Uani d . 1 . . P P3 0.68651(4) 1.04620(5) 0.14519(3) 0.01593(13) Uani d . 1 . . P P4 0.52714(4) 0.78683(5) 0.05567(3) 0.01727(13) Uani d . 1 . . P P5 0.78963(5) 0.61096(5) 0.04647(3) 0.01956(14) Uani d . 1 . . P P6 0.23020(4) 0.63720(5) 0.13206(3) 0.01714(13) Uani d . 1 . . P O1 0.82104(13) 0.96239(14) -0.14012(10) 0.0235(4) Uani d . 1 . . O O2 0.78353(13) 1.01609(13) -0.01967(9) 0.0208(4) Uani d . 1 . . O O3 0.70998(14) 0.84849(15) -0.07304(10) 0.0254(4) Uani d . 1 . . O O4 0.65465(15) 1.03185(18) -0.11871(11) 0.0329(5) Uani d . 1 . . O H41 0.6168 1.0449 -0.0889 0.049 Uiso calc R 1 . . H O5 0.90059(12) 0.92684(15) 0.05752(10) 0.0230(4) Uani d . 1 . . O O6 1.00231(13) 0.76595(16) 0.09603(12) 0.0322(5) Uani d . 1 . . O O7 0.86254(12) 0.83116(16) 0.16704(10) 0.0249(4) Uani d . 1 . . O O8 1.01490(14) 0.93903(17) 0.16472(11) 0.0302(4) Uani d . 1 . . O H81 1.0656 0.9493 0.1450 0.045 Uiso calc R 1 . . H O9 0.70167(13) 1.14126(13) 0.19431(9) 0.0210(4) Uani d . 1 . . O O10 0.77572(13) 1.04328(13) 0.09928(10) 0.0216(4) Uani d . 1 . . O O11 0.67750(13) 0.93840(14) 0.18215(10) 0.0229(4) Uani d . 1 . . O O12 0.58899(14) 1.07296(16) 0.10113(11) 0.0294(4) Uani d . 1 . . O H121 0.5669 1.0170 0.0828 0.044 Uiso calc R 1 . . H O13 0.57789(13) 0.75713(16) 0.12460(10) 0.0262(4) Uani d . 1 . . O O14 0.59685(13) 0.76145(17) -0.00221(10) 0.0275(4) Uani d . 1 . . O O15 0.48945(14) 0.90274(16) 0.05260(12) 0.0317(5) Uani d . 1 . . O O16 0.44099(14) 0.70462(17) 0.03714(10) 0.0304(4) Uani d . 1 . . O H161 0.4129 0.6896 0.0716 0.046 Uiso calc R 1 . . H O17 0.76581(16) 0.69934(15) -0.00856(10) 0.0305(4) Uani d . 1 . . O O18 0.74692(18) 0.50114(16) 0.02499(12) 0.0409(6) Uani d . 1 . . O O19 0.75430(16) 0.64764(14) 0.11394(10) 0.0300(4) Uani d . 1 . . O O20 0.90470(15) 0.59582(19) 0.05141(13) 0.0414(6) Uani d . 1 . . O H201 0.9317 0.6547 0.0600 0.062 Uiso calc R 1 . . H O21 0.72902(12) 0.86664(13) 0.05172(9) 0.0175(3) Uani d . 1 . . O O22 0.71480(14) 0.73386(15) 0.23475(10) 0.0242(4) Uani d . 1 . . O O23 0.34197(12) 0.64073(15) 0.13645(11) 0.0264(4) Uani d . 1 . . O O24 0.19049(17) 0.5908(3) 0.19777(13) 0.0604(9) Uani d . 1 . . O H24 0.2310 0.6023 0.2301 0.091 Uiso calc R 1 . . H O25 0.18085(19) 0.5662(3) 0.07675(14) 0.0564(8) Uani d . 1 . . O H25 0.2155 0.5640 0.0441 0.085 Uiso calc R 1 . . H O26 0.19260(17) 0.7542(2) 0.1237(2) 0.0764(11) Uani d . 1 . . O H26 0.1364 0.7538 0.1047 0.115 Uiso calc R 1 . . H O27 0.80419(19) 0.49715(19) 0.21476(13) 0.0406(6) Uani d . 1 . . O H27A 0.805(3) 0.506(4) 0.257(3) 0.061 Uiso d . 1 . . H H27B 0.787(3) 0.556(4) 0.194(2) 0.061 Uiso d . 1 . . H N1 0.57059(14) 0.30495(16) 0.18197(11) 0.0183(4) Uani d . 1 . . N H1 0.6080 0.2438 0.1898 0.022 Uiso calc R 1 . . H N2 0.46899(16) 0.47310(17) 0.16013(12) 0.0245(5) Uani d . 1 . . N H2 0.4320 0.5345 0.1524 0.029 Uiso calc R 1 . . H C1 0.40085(18) 0.3763(2) 0.16156(16) 0.0267(6) Uani d . 1 . . C H1A 0.3568 0.3745 0.1203 0.032 Uiso calc R 1 . . H H1B 0.3606 0.3814 0.2005 0.032 Uiso calc R 1 . . H C2 0.6077(2) 0.3651(2) 0.12248(15) 0.0268(6) Uani d . 1 . . C H2A 0.6103 0.3163 0.0838 0.032 Uiso calc R 1 . . H H2B 0.6742 0.3925 0.1342 0.032 Uiso calc R 1 . . H C3 0.46439(19) 0.2723(2) 0.16676(17) 0.0278(6) Uani d . 1 . . C H3A 0.4429 0.2257 0.2029 0.033 Uiso calc R 1 . . H H3B 0.4572 0.2322 0.1241 0.033 Uiso calc R 1 . . H C4 0.5790(2) 0.3747(2) 0.24460(15) 0.0302(6) Uani d . 1 . . C H4A 0.6484 0.3860 0.2594 0.036 Uiso calc R 1 . . H H4B 0.5467 0.3394 0.2813 0.036 Uiso calc R 1 . . H C5 0.5290(2) 0.4839(2) 0.22713(17) 0.0321(6) Uani d . 1 . . C H5A 0.4862 0.5043 0.2627 0.039 Uiso calc R 1 . . H H5B 0.5790 0.5403 0.2240 0.039 Uiso calc R 1 . . H C6 0.5376(2) 0.4598(2) 0.10401(17) 0.0337(7) Uani d . 1 . . C H6A 0.5754 0.5262 0.0988 0.040 Uiso calc R 1 . . H H6B 0.4997 0.4448 0.0612 0.040 Uiso calc R 1 . . H N3 -0.05811(18) 0.71573(19) 0.35649(13) 0.0298(5) Uani d . 1 . . N H3 -0.1059 0.6633 0.3566 0.036 Uiso calc R 1 . . H N4 0.07089(18) 0.8594(2) 0.35558(16) 0.0378(6) Uani d . 1 . . N H4 0.1184 0.9120 0.3553 0.045 Uiso calc R 1 . . H B1 0.79514(19) 0.9607(2) 0.04696(14) 0.0164(5) Uani d . 1 . . B B2 0.70014(19) 0.7974(2) -0.00588(14) 0.0163(5) Uani d . 1 . . B C7 0.0040(3) 0.6962(2) 0.29747(18) 0.0404(8) Uani d . 1 . . C H7A -0.0361 0.7045 0.2548 0.049 Uiso calc R 1 . . H H7B 0.0307 0.6226 0.2995 0.049 Uiso calc R 1 . . H C8 -0.1073(2) 0.8252(3) 0.34921(17) 0.0345(6) Uani d . 1 . . C H8A -0.1439 0.8402 0.3890 0.041 Uiso calc R 1 . . H H8B -0.1539 0.8258 0.3092 0.041 Uiso calc R 1 . . H C9 0.0881(2) 0.7787(3) 0.3015(2) 0.0414(8) Uani d . 1 . . C H9A 0.1510 0.7418 0.3119 0.050 Uiso calc R 1 . . H H9B 0.0909 0.8154 0.2579 0.050 Uiso calc R 1 . . H C10 0.0051(3) 0.7097(3) 0.42208(18) 0.0422(8) Uani d . 1 . . C H10A 0.0411 0.6412 0.4249 0.051 Uiso calc R 1 . . H H10B -0.0360 0.7143 0.4605 0.051 Uiso calc R 1 . . H C11 0.0780(3) 0.8053(4) 0.4234(2) 0.0577(11) Uani d . 1 . . C H11A 0.0621 0.8571 0.4584 0.069 Uiso calc R 1 . . H H11B 0.1452 0.7791 0.4340 0.069 Uiso calc R 1 . . H C12 -0.0287(2) 0.9114(3) 0.3423(2) 0.0499(10) Uani d . 1 . . C H12A -0.0347 0.9422 0.2967 0.060 Uiso calc R 1 . . H H12B -0.0368 0.9697 0.3749 0.060 Uiso calc R 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 V1 0.01776(19) 0.01314(17) 0.0130(2) 0.00111(13) 0.00357(14) 0.00006(13) P1 0.0153(3) 0.0202(3) 0.0152(3) 0.0021(2) 0.0032(2) 0.0048(2) P2 0.0126(3) 0.0221(3) 0.0223(4) 0.0029(2) 0.0009(2) 0.0011(2) P3 0.0168(3) 0.0135(3) 0.0178(3) 0.0022(2) 0.0031(2) -0.0031(2) P4 0.0130(3) 0.0221(3) 0.0171(3) -0.0029(2) 0.0038(2) -0.0009(2) P5 0.0259(3) 0.0148(3) 0.0188(4) 0.0029(2) 0.0074(2) -0.0030(2) P6 0.0130(3) 0.0200(3) 0.0188(3) 0.0009(2) 0.0038(2) -0.0014(2) O1 0.0230(9) 0.0248(9) 0.0239(11) -0.0006(7) 0.0102(7) 0.0015(7) O2 0.0286(9) 0.0169(8) 0.0167(9) -0.0029(7) 0.0004(7) 0.0045(6) O3 0.0354(10) 0.0247(9) 0.0159(10) -0.0107(7) 0.0009(7) 0.0037(7) O4 0.0281(10) 0.0471(12) 0.0235(11) 0.0175(9) 0.0018(8) 0.0080(9) O5 0.0161(8) 0.0313(9) 0.0221(10) 0.0043(7) 0.0047(6) 0.0065(7) O6 0.0177(9) 0.0276(10) 0.0512(14) 0.0088(7) 0.0028(8) -0.0028(9) O7 0.0171(8) 0.0348(10) 0.0224(11) -0.0012(7) 0.0002(7) 0.0076(8) O8 0.0205(9) 0.0423(11) 0.0280(12) -0.0088(8) 0.0036(7) -0.0063(9) O9 0.0269(9) 0.0165(8) 0.0195(10) 0.0049(6) -0.0008(7) -0.0052(6) O10 0.0244(9) 0.0179(8) 0.0234(10) -0.0026(6) 0.0085(7) -0.0041(7) O11 0.0301(9) 0.0160(8) 0.0239(10) 0.0032(7) 0.0106(7) -0.0002(7) O12 0.0255(9) 0.0250(9) 0.0363(12) 0.0045(7) -0.0081(8) -0.0065(8) O13 0.0223(9) 0.0333(10) 0.0225(11) -0.0093(7) -0.0011(7) 0.0057(7) O14 0.0182(8) 0.0427(11) 0.0226(11) -0.0101(8) 0.0075(7) -0.0088(8) O15 0.0216(9) 0.0275(10) 0.0458(14) 0.0054(7) 0.0002(8) -0.0011(9) O16 0.0236(9) 0.0428(11) 0.0253(11) -0.0187(8) 0.0059(7) -0.0040(8) O17 0.0448(12) 0.0275(10) 0.0204(11) 0.0144(8) 0.0091(8) -0.0001(7) O18 0.0613(14) 0.0228(10) 0.0424(14) -0.0152(9) 0.0309(11) -0.0145(9) O19 0.0566(13) 0.0168(8) 0.0179(11) 0.0090(8) 0.0120(8) -0.0007(7) O20 0.0279(10) 0.0380(12) 0.0580(16) 0.0110(9) 0.0000(10) -0.0174(11) O21 0.0200(8) 0.0172(8) 0.0155(9) -0.0035(6) 0.0025(6) 0.0010(6) O22 0.0322(10) 0.0243(9) 0.0167(10) 0.0024(7) 0.0070(7) 0.0019(7) O23 0.0142(8) 0.0298(10) 0.0358(12) 0.0052(7) 0.0065(7) 0.0094(8) O24 0.0326(12) 0.125(3) 0.0235(14) -0.0378(14) -0.0002(9) 0.0155(14) O25 0.0429(13) 0.085(2) 0.0431(17) -0.0204(13) 0.0183(11) -0.0418(14) O26 0.0212(11) 0.0244(11) 0.182(4) 0.0070(9) -0.0037(16) 0.0134(16) O27 0.0602(15) 0.0323(11) 0.0291(13) 0.0194(10) 0.0019(10) 0.0007(9) N1 0.0184(9) 0.0166(9) 0.0197(11) 0.0050(7) 0.0009(7) -0.0004(7) N2 0.0205(10) 0.0193(10) 0.0344(14) 0.0060(8) 0.0075(9) 0.0030(9) C1 0.0171(11) 0.0249(12) 0.0382(17) 0.0009(9) 0.0027(10) 0.0020(11) C2 0.0262(13) 0.0319(14) 0.0237(15) 0.0068(10) 0.0118(10) 0.0024(10) C3 0.0190(12) 0.0209(12) 0.0433(18) -0.0019(9) 0.0012(11) -0.0010(11) C4 0.0380(15) 0.0307(14) 0.0215(16) 0.0036(11) -0.0015(11) -0.0072(11) C5 0.0291(14) 0.0274(13) 0.0401(18) 0.0036(11) 0.0052(12) -0.0138(12) C6 0.0351(15) 0.0320(14) 0.0357(18) 0.0082(12) 0.0155(12) 0.0137(12) N3 0.0333(12) 0.0299(12) 0.0271(14) -0.0146(9) 0.0088(10) -0.0036(9) N4 0.0233(11) 0.0228(11) 0.068(2) -0.0050(9) 0.0106(11) -0.0034(11) B1 0.0175(12) 0.0160(11) 0.0162(14) -0.0004(9) 0.0035(9) 0.0005(9) B2 0.0157(11) 0.0197(12) 0.0139(14) 0.0009(9) 0.0041(9) 0.0008(9) C7 0.058(2) 0.0294(15) 0.037(2) -0.0068(13) 0.0237(15) -0.0078(12) C8 0.0234(13) 0.0421(16) 0.0381(19) 0.0021(12) 0.0033(11) 0.0001(13) C9 0.0385(17) 0.0365(16) 0.052(2) 0.0041(13) 0.0246(15) 0.0046(14) C10 0.060(2) 0.0374(17) 0.0287(19) -0.0018(15) -0.0016(14) 0.0057(13) C11 0.052(2) 0.070(3) 0.048(3) -0.0164(19) -0.0158(17) -0.0132(19) C12 0.0315(16) 0.0265(15) 0.094(3) 0.0082(12) 0.0169(17) -0.0003(16) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag V1 O22 . 1.6026(19) y V1 O11 . 1.9944(17) y V1 O13 . 2.0043(18) y V1 O19 . 2.0079(18) y V1 O7 . 2.0159(17) y V1 O21 . 2.3592(17) y P1 O1 . 1.5107(18) y P1 O4 . 1.5350(19) y P1 O2 . 1.5376(19) y P1 O3 . 1.5454(18) y P2 O6 . 1.5147(19) y P2 O7 . 1.5149(18) y P2 O5 . 1.5493(19) y P2 O8 . 1.572(2) y P3 O11 . 1.5164(18) y P3 O9 . 1.5168(17) y P3 O10 . 1.5546(18) y P3 O12 . 1.5564(19) y P4 O15 . 1.509(2) y P4 O13 . 1.516(2) y P4 O14 . 1.5570(19) y P4 O16 . 1.5612(18) y P5 O19 . 1.5077(19) y P5 O18 . 1.512(2) y P5 O17 . 1.547(2) y P5 O20 . 1.559(2) y P6 O23 . 1.5045(18) y P6 O25 . 1.509(2) y P6 O26 . 1.526(2) y P6 O24 . 1.540(2) y O2 B1 . 1.472(3) y O3 B2 . 1.474(3) y O4 H41 . 0.8200 ? O5 B1 . 1.482(3) y O8 H81 . 0.8200 ? O10 B1 . 1.478(3) y O12 H121 . 0.8200 ? O14 B2 . 1.468(3) y O16 H161 . 0.8200 ? O17 B2 . 1.497(3) y O20 H201 . 0.8200 ? O21 B2 . 1.444(3) y O21 B1 . 1.465(3) y O24 H24 . 0.8200 ? O25 H25 . 0.8200 ? O26 H26 . 0.8200 ? O27 H27A . 0.83(5) ? O27 H27B . 0.85(5) ? N1 C4 . 1.495(3) ? N1 C3 . 1.497(3) ? N1 C2 . 1.497(3) ? N1 H1 . 0.9100 ? N2 C6 . 1.498(3) ? N2 C5 . 1.500(4) ? N2 C1 . 1.502(3) ? N2 H2 . 0.9100 ? C1 C3 . 1.536(4) ? C1 H1A . 0.9700 ? C1 H1B . 0.9700 ? C2 C6 . 1.523(4) ? C2 H2A . 0.9700 ? C2 H2B . 0.9700 ? C3 H3A . 0.9700 ? C3 H3B . 0.9700 ? C4 C5 . 1.527(4) ? C4 H4A . 0.9700 ? C4 H4B . 0.9700 ? C5 H5A . 0.9700 ? C5 H5B . 0.9700 ? C6 H6A . 0.9700 ? C6 H6B . 0.9700 ? N3 C10 . 1.494(4) ? N3 C7 . 1.497(4) ? N3 C8 . 1.499(4) ? N3 H3 . 0.9100 ? N4 C9 . 1.482(4) ? N4 C11 . 1.483(5) ? N4 C12 . 1.492(4) ? N4 H4 . 0.9100 ? C7 C9 . 1.518(4) ? C7 H7A . 0.9700 ? C7 H7B . 0.9700 ? C8 C12 . 1.510(4) ? C8 H8A . 0.9700 ? C8 H8B . 0.9700 ? C9 H9A . 0.9700 ? C9 H9B . 0.9700 ? C10 C11 . 1.528(5) ? C10 H10A . 0.9700 ? C10 H10B . 0.9700 ? C11 H11A . 0.9700 ? C11 H11B . 0.9700 ? C12 H12A . 0.9700 ? C12 H12B . 0.9700 ?