#------------------------------------------------------------------------------ #$Date: 2011-09-28 15:24:46 +0100 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: svn://www.crystallography.net/cod/cif/2/00/32/2003229.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_2003229 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _journal_page_first 353 _journal_page_last 356 _publ_section_title ; Hydrogen-Bonded Self-Assembly of Tris(2-aminoethyl)amine Molybdate Hydrate, 4[N(CH~2~CH~2~NH~3~)~3~]^3+^.6[MoO~4~]^2-^.6H~2~O ; _chemical_formula_moiety '4(C6 H21 N4) 6[Mo O4], 6H2 O' _chemical_formula_sum 'C24 H96 Mo6 N16 O30' _chemical_formula_weight 1664.74 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 1/2-x,1/2+y,1/2-z 1/2+x,1/2-y,1/2+z _cell_length_a 16.374(2) _cell_length_b 20.082(2) _cell_length_c 19.137(5) _cell_angle_alpha 90.0 _cell_angle_beta 90.610(10) _cell_angle_gamma 90.0 _cell_volume 6292(2) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.757 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _diffrn_radiation_type 'Molybdenum K\a' _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.00 _cell_measurement_theta_max 20.50 _exptl_absorpt_coefficient_mu 1.22 _cell_measurement_temperature 293 _exptl_crystal_description 'Block' _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.24 _exptl_crystal_size_rad ? _exptl_crystal_colour 'colourless' _chemical_compound_source 'synthesised by the authors' _diffrn_measurement_device 'Enraf-Nonius CAD-4' _diffrn_measurement_method '\q/2\q scan b/P/b ' _exptl_absorpt_correction_type 'empirical, 9 \y scans, 4\% steps' _exptl_absorpt_correction_T_min 0.4951 _exptl_absorpt_correction_T_max 0.6200 _diffrn_reflns_number 14084 _reflns_number_total 13688 _reflns_number_observed 11057 _reflns_observed_criterion 'Inet > 3.0\s(Inet)' _diffrn_reflns_av_R_equivalents 0.018 _diffrn_reflns_theta_max 26.92 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 2.5 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs 0.030 _refine_ls_wR_factor_obs 0.045 _refine_ls_wR_factor_all 0.049 _refine_ls_goodness_of_fit_obs 1.25 _refine_ls_goodness_of_fit_all ? _refine_ls_number_reflns 11057 _refine_ls_number_parameters 686 _refine_ls_hydrogen_treatment 'C-H, N-H and O-H = 0.95\%A' _refine_ls_weighting_scheme '1/[\s^2^(F) + 0.0008F^2^]' _refine_ls_shift/esd_max 0.007 _refine_diff_density_max 0.85 _refine_diff_density_min -0.73 _refine_ls_extinction_method 'Larson (1970)' _refine_ls_extinction_coef 2472(314) loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Mo1 0.931156(17) 0.623716(14) 0.172448(14) 0.02435(14) Mo2 1.121308(17) 0.825520(14) 0.324736(14) 0.02683(14) Mo3 0.070855(17) 0.392634(14) 0.328724(14) 0.02698(13) Mo4 0.602725(17) 0.662489(14) 0.332493(14) 0.02667(13) Mo5 0.290510(16) 0.605330(13) 0.269584(14) 0.02462(13) Mo6 0.730397(16) 0.387883(13) 0.226262(15) 0.02476(12) O11 0.93392(16) 0.62361(13) 0.26564(12) 0.0396(14) O12 0.84946(16) 0.67307(15) 0.14424(15) 0.0520(15) O13 1.02158(16) 0.65678(15) 0.14075(15) 0.0523(15) O14 0.9180(2) 0.54328(14) 0.14220(15) 0.0619(19) O21 1.11853(17) 0.83144(13) 0.23236(12) 0.0445(14) O22 1.19033(16) 0.88370(12) 0.36049(14) 0.0451(14) O23 1.1504(2) 0.74540(13) 0.34872(17) 0.070(2) O24 1.02439(18) 0.83987(17) 0.35495(17) 0.0691(19) O31 0.07991(17) 0.38274(13) 0.23692(12) 0.0414(14) O32 -0.00736(19) 0.44638(19) 0.34851(19) 0.081(2) O33 0.16025(18) 0.4262(2) 0.36264(17) 0.088(3) O34 0.0510(3) 0.31773(17) 0.36805(18) 0.105(3) O41 0.59605(16) 0.65477(13) 0.23964(12) 0.0399(14) O42 0.53216(17) 0.72042(14) 0.36103(15) 0.0530(15) O43 0.5808(2) 0.58578(14) 0.37115(15) 0.063(2) O44 0.69974(17) 0.68671(18) 0.35770(17) 0.071(2) O51 0.31600(15) 0.68367(12) 0.23432(13) 0.0396(13) O52 0.2945(2) 0.60795(16) 0.35910(15) 0.067(2) O53 0.19136(14) 0.58371(13) 0.24095(14) 0.0421(13) O54 0.35773(17) 0.54360(14) 0.23901(15) 0.0548(16) O61 0.71739(15) 0.46592(11) 0.26805(13) 0.0374(13) O62 0.65988(14) 0.32783(12) 0.25576(13) 0.0377(12) O63 0.7226(2) 0.39946(15) 0.13723(14) 0.0579(18) O64 0.82801(14) 0.35754(13) 0.24772(14) 0.0445(14) O1 0.63750(18) 0.46184(14) 0.40043(14) 0.0518(16) O2 0.3642(2) 0.50795(14) 0.09851(15) 0.0584(19) O3 0.9664(2) 0.95917(18) 0.4086(2) 0.090(3) O4 0.7191(2) 0.39589(16) -0.00812(17) 0.069(2) O5 0.5022(2) 0.48762(17) 0.2867(3) 0.105(3) O6 0.2742(2) 0.61820(18) 0.50301(16) 0.074(2) N1 0.93192(15) 0.62174(13) 0.43420(13) 0.0251(12) N11 0.85871(17) 0.72417(15) 0.34134(16) 0.0377(15) N12 0.85642(16) 0.51995(13) 0.33863(14) 0.0320(13) N13 1.07924(16) 0.62150(14) 0.34323(15) 0.0327(13) N2 1.10646(16) 0.83586(13) 0.06286(14) 0.0283(13) N21 0.97021(17) 0.85117(15) 0.16055(15) 0.0366(15) N22 1.16994(18) 0.72482(15) 0.15513(16) 0.0392(15) N23 1.17979(18) 0.93798(15) 0.15607(17) 0.0424(16) N3 0.07533(15) 0.38332(12) 0.06285(13) 0.0239(12) N31 0.12073(18) 0.27060(14) 0.15673(15) 0.0363(15) N32 0.17427(17) 0.46990(13) 0.15964(15) 0.0325(13) N33 -0.06181(16) 0.40760(14) 0.15611(15) 0.0349(14) N4 0.61183(15) 0.66288(13) 0.06893(13) 0.0251(13) N41 0.6426(2) 0.54463(14) 0.16104(16) 0.0424(17) N42 0.70428(19) 0.74222(14) 0.17056(15) 0.0390(15) N43 0.46302(17) 0.68812(16) 0.15706(16) 0.0419(16) C1A 0.8811(2) 0.67731(17) 0.45856(16) 0.0296(16) C2A 0.8895(2) 0.73815(17) 0.41314(19) 0.0371(18) C3A 0.8984(2) 0.55729(16) 0.45689(17) 0.0312(16) C4A 0.8280(2) 0.53449(18) 0.41017(19) 0.0360(17) C5A 1.0167(2) 0.62958(18) 0.45960(17) 0.0326(16) C6A 1.07722(19) 0.59232(17) 0.41437(19) 0.0339(17) C1B 1.0217(2) 0.84730(18) 0.03996(17) 0.0354(17) C2B 0.9620(2) 0.81775(17) 0.0918(2) 0.0362(18) C3B 1.1352(2) 0.76992(18) 0.03892(17) 0.0356(18) C4B 1.2022(2) 0.74146(18) 0.08526(19) 0.0400(18) C5B 1.1614(2) 0.88917(18) 0.03918(19) 0.0399(18) C6B 1.1522(3) 0.95090(19) 0.0844(2) 0.049(2) C1C 0.0941(2) 0.31569(16) 0.03872(16) 0.0289(15) C2C 0.1547(2) 0.28050(17) 0.08519(19) 0.0354(17) C3C 0.13805(19) 0.43121(16) 0.04044(16) 0.0291(15) C4C 0.1437(2) 0.49022(17) 0.08990(19) 0.0356(17) C5C -0.00619(19) 0.40475(16) 0.03832(16) 0.0298(16) C6C -0.07244(19) 0.37885(17) 0.08551(19) 0.0334(18) C1D 0.6343(2) 0.59641(17) 0.04487(18) 0.0347(17) C2D 0.6889(2) 0.56124(17) 0.0973(2) 0.0407(19) C3D 0.6739(2) 0.71237(17) 0.04885(17) 0.0338(17) C4D 0.6783(2) 0.76880(18) 0.1014(2) 0.0412(19) C5D 0.5306(2) 0.68356(18) 0.04265(17) 0.0350(17) C6D 0.4622(2) 0.65639(18) 0.0874(2) 0.041(2) H11a 0.864 0.763 0.313 0.0477 H11b 0.890 0.689 0.322 0.0477 H11c 0.803 0.712 0.343 0.0477 H12a 0.811 0.506 0.311 0.0420 H12b 0.879 0.559 0.319 0.0420 H12c 0.896 0.486 0.340 0.0420 H13a 1.117 0.598 0.316 0.0427 H13b 1.026 0.619 0.322 0.0427 H13c 1.095 0.667 0.346 0.0427 H21a 0.933 0.832 0.192 0.0466 H21b 1.024 0.845 0.178 0.0466 H21c 0.959 0.897 0.155 0.0466 H22a 1.213 0.707 0.184 0.0492 H22b 1.149 0.764 0.176 0.0492 H22c 1.128 0.693 0.150 0.0492 H23a 1.174 0.977 0.184 0.0524 H23b 1.149 0.903 0.176 0.0524 H23c 1.236 0.925 0.156 0.0524 H31a 0.160 0.248 0.185 0.0462 H31b 0.108 0.313 0.177 0.0462 H31c 0.072 0.244 0.153 0.0462 H32a 0.177 0.508 0.189 0.0425 H32b 0.138 0.438 0.179 0.0425 H32c 0.227 0.451 0.156 0.0425 H33a -0.104 0.391 0.186 0.0450 H33b -0.010 0.395 0.175 0.0450 H33c -0.065 0.455 0.153 0.0450 H41a 0.678 0.523 0.193 0.0524 H41b 0.623 0.584 0.182 0.0524 H41c 0.598 0.516 0.149 0.0524 H42a 0.707 0.778 0.203 0.0489 H42b 0.666 0.710 0.185 0.0489 H42c 0.756 0.722 0.167 0.0489 H43a 0.420 0.671 0.184 0.0519 H43b 0.514 0.680 0.180 0.0519 H43c 0.456 0.735 0.152 0.0519 H1Aa 0.826 0.664 0.459 0.0396 H1Ab 0.898 0.689 0.505 0.0396 H2Aa 0.945 0.751 0.411 0.0471 H2Ab 0.859 0.774 0.433 0.0471 H3Aa 0.940 0.525 0.455 0.0412 H3Ab 0.879 0.561 0.503 0.0412 H4Aa 0.788 0.568 0.408 0.0460 H4Ab 0.805 0.495 0.429 0.0460 H5Aa 1.030 0.676 0.459 0.0425 H5Ab 1.021 0.613 0.506 0.0425 H6Aa 1.061 0.547 0.411 0.0438 H6Ab 1.130 0.595 0.435 0.0438 H1Ba 1.012 0.894 0.036 0.0453 H1Bb 1.013 0.827 -0.004 0.0453 H2Ba 0.973 0.772 0.097 0.0462 H2Bb 0.908 0.824 0.075 0.0462 H3Ba 1.090 0.740 0.039 0.0456 H3Bb 1.155 0.774 -0.007 0.0456 H4Ba 1.245 0.773 0.090 0.0500 H4Bb 1.223 0.702 0.064 0.0500 H5Ba 1.216 0.874 0.042 0.0499 H5Bb 1.149 0.900 -0.008 0.0499 H6Ba 1.096 0.963 0.084 0.0587 H6Bb 1.184 0.986 0.065 0.0587 H1Ca 0.045 0.291 0.037 0.0389 H1Cb 0.116 0.318 -0.007 0.0389 H2Ca 0.203 0.306 0.089 0.0454 H2Cb 0.168 0.238 0.066 0.0454 H3Ca 0.190 0.409 0.039 0.0391 H3Cb 0.124 0.447 -0.005 0.0391 H4Ca 0.091 0.510 0.095 0.0455 H4Cb 0.180 0.522 0.071 0.0455 H5Ca -0.008 0.452 0.038 0.0397 H5Cb -0.015 0.388 -0.008 0.0397 H6Ca -0.069 0.332 0.088 0.0435 H6Cb -0.124 0.391 0.067 0.0435 H1Da 0.586 0.571 0.038 0.0447 H1Db 0.662 0.600 0.002 0.0447 H2Da 0.734 0.589 0.109 0.0506 H2Db 0.709 0.522 0.077 0.0506 H3Da 0.726 0.691 0.047 0.0439 H3Db 0.660 0.730 0.004 0.0439 H4Da 0.626 0.789 0.105 0.0512 H4Db 0.717 0.801 0.086 0.0512 H5Da 0.528 0.731 0.043 0.0449 H5Db 0.523 0.668 -0.004 0.0449 H6Da 0.469 0.610 0.093 0.0514 H6Db 0.411 0.665 0.065 0.0514 H1W1 0.618 0.505 0.390 0.0618 H2W1 0.664 0.464 0.356 0.0618 H1W2 0.362 0.520 0.147 0.0684 H2W2 0.345 0.465 0.113 0.0684 H1W3 0.987 0.919 0.390 0.0998 H2W3 1.021 0.974 0.406 0.0998 H1W4 0.720 0.397 0.041 0.0791 H2W4 0.692 0.428 -0.037 0.0791 H1W5 0.528 0.521 0.315 0.1146 H2W5 0.452 0.507 0.271 0.1146 H1W6 0.281 0.615 0.454 0.0841 H2W6 0.304 0.591 0.535 0.0841 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 Mo1 0.0301(2) -0.00081(10) 0.00073(10) 0.0247(2) 0.00046(10) 0.0183(2) Mo2 0.0343(2) -0.00375(11) -0.00067(11) 0.0250(2) 0.00032(11) 0.0211(2) Mo3 0.0311(2) 0.00302(11) 0.00104(11) 0.0306(2) -0.00255(11) 0.0192(2) Mo4 0.0297(2) 0.00430(11) -0.00002(10) 0.0307(2) -0.00181(11) 0.0196(2) Mo5 0.0279(2) 0.00124(10) 0.00069(11) 0.0218(2) -0.00134(10) 0.0243(2) Mo6 0.0249(2) 0.00036(10) 0.00272(10) 0.0230(2) 0.00315(10) 0.0264(2) O11 0.047(2) -0.0004(12) 0.0002(10) 0.052(2) 0.0017(11) 0.0197(12) O12 0.040(2) 0.0089(13) -0.0070(13) 0.059(2) 0.0119(14) 0.056(2) O13 0.042(2) -0.0082(13) 0.0145(13) 0.063(2) 0.0115(14) 0.052(2) O14 0.096(3) -0.003(2) -0.009(2) 0.034(2) -0.0122(14) 0.055(2) O21 0.056(2) 0.0046(13) -0.0008(11) 0.053(2) -0.0023(11) 0.0241(12) O22 0.051(2) -0.0098(12) -0.0120(13) 0.0340(14) 0.0000(12) 0.050(2) O23 0.104(3) -0.005(2) -0.032(2) 0.032(2) 0.012(2) 0.074(2) O24 0.050(2) -0.013(2) 0.027(2) 0.085(2) -0.007(2) 0.073(2) O31 0.053(2) -0.0070(12) 0.0045(11) 0.049(2) 0.0004(11) 0.0220(12) O32 0.052(2) 0.035(2) -0.003(2) 0.100(3) -0.042(2) 0.089(3) O33 0.037(2) -0.015(2) -0.001(2) 0.160(4) -0.051(2) 0.067(2) O34 0.220(5) -0.019(3) 0.015(3) 0.048(2) 0.009(2) 0.048(2) O41 0.051(2) 0.0015(12) -0.0007(11) 0.0430(14) 0.0015(11) 0.0257(12) O42 0.052(2) 0.0168(14) 0.0101(13) 0.054(2) -0.0124(14) 0.053(2) O43 0.112(3) 0.002(2) -0.002(2) 0.037(2) 0.0100(13) 0.040(2) O44 0.037(2) -0.009(2) -0.009(2) 0.113(3) -0.012(2) 0.064(2) O51 0.0370(13) -0.0070(10) 0.0016(11) 0.0327(13) 0.0086(11) 0.049(2) O52 0.095(3) 0.014(2) -0.003(2) 0.078(2) 0.0046(14) 0.029(2) O53 0.0323(13) -0.0077(11) 0.0051(11) 0.0397(14) -0.0200(12) 0.054(2) O54 0.051(2) 0.0232(14) -0.0069(14) 0.053(2) -0.0174(14) 0.060(2) O61 0.0405(14) -0.0013(10) -0.0053(11) 0.0276(12) -0.0019(11) 0.044(2) O62 0.0339(13) -0.0069(10) 0.0111(11) 0.0311(13) -0.0056(11) 0.048(2) O63 0.080(2) 0.016(2) 0.0032(14) 0.062(2) 0.0069(13) 0.031(2) O64 0.0270(12) 0.0066(11) 0.0095(11) 0.049(2) 0.0255(13) 0.058(2) O1 0.062(2) -0.0004(14) 0.0013(14) 0.048(2) 0.0080(13) 0.045(2) O2 0.089(2) -0.008(2) 0.005(2) 0.040(2) 0.0014(13) 0.047(2) O3 0.072(2) 0.025(2) -0.008(2) 0.070(2) -0.012(2) 0.127(4) O4 0.089(3) 0.017(2) -0.007(2) 0.075(2) -0.005(2) 0.043(2) O5 0.077(3) -0.002(2) -0.065(3) 0.054(2) 0.014(2) 0.183(4) O6 0.097(3) 0.035(2) -0.001(2) 0.089(3) -0.006(2) 0.037(2) N1 0.0264(13) -0.0015(10) 0.0010(10) 0.0282(14) -0.0026(10) 0.0208(13) N11 0.036(2) 0.0077(13) 0.0050(13) 0.036(2) 0.0103(13) 0.041(2) N12 0.033(2) -0.0054(12) -0.0033(12) 0.031(2) -0.0050(12) 0.032(2) N13 0.0290(14) -0.0040(11) 0.0074(12) 0.034(2) -0.0068(12) 0.035(2) N2 0.0317(14) -0.0031(11) 0.0017(11) 0.032(2) -0.0007(11) 0.0216(13) N21 0.030(2) 0.0024(12) 0.0089(12) 0.039(2) 0.0026(13) 0.041(2) N22 0.040(2) 0.0128(13) -0.0031(13) 0.039(2) 0.0051(13) 0.039(2) N23 0.038(2) -0.0071(13) 0.0021(14) 0.039(2) -0.014(2) 0.051(2) N3 0.0250(13) -0.0006(10) 0.0009(10) 0.0249(13) 0.0012(10) 0.0219(13) N31 0.043(2) -0.0015(12) -0.0095(13) 0.0265(14) 0.0040(12) 0.039(2) N32 0.036(2) -0.0053(12) 0.0007(12) 0.029(2) -0.0070(12) 0.033(2) N33 0.0278(14) 0.0018(12) 0.0121(12) 0.039(2) 0.0033(13) 0.038(2) N4 0.0294(14) 0.0004(10) 0.0013(10) 0.0257(13) 0.0007(10) 0.0201(13) N41 0.061(2) 0.0097(14) -0.010(2) 0.027(2) 0.0035(13) 0.039(2) N42 0.048(2) -0.0118(13) 0.0003(13) 0.032(2) -0.0105(13) 0.037(2) N43 0.027(2) 0.0025(13) 0.0082(13) 0.054(2) 0.012(2) 0.045(2) C1A 0.032(2) 0.0016(13) 0.0020(13) 0.035(2) -0.0029(13) 0.022(2) C2A 0.041(2) 0.0012(14) 0.002(2) 0.029(2) -0.001(2) 0.041(2) C3A 0.036(2) -0.0033(14) 0.0017(13) 0.030(2) 0.0046(13) 0.027(2) C4A 0.031(2) -0.0093(14) 0.0051(14) 0.039(2) -0.001(2) 0.038(2) C5A 0.030(2) -0.0040(14) -0.0031(13) 0.043(2) -0.0051(14) 0.025(2) C6A 0.024(2) 0.0021(13) -0.0006(14) 0.037(2) -0.004(2) 0.040(2) C1B 0.039(2) -0.002(2) -0.0046(14) 0.040(2) 0.007(2) 0.028(2) C2B 0.026(2) -0.0027(14) -0.002(2) 0.037(2) 0.004(2) 0.046(2) C3B 0.046(2) 0.000(2) 0.0025(14) 0.037(2) -0.0070(14) 0.023(2) C4B 0.040(2) 0.007(2) 0.0010(2) 0.040(2) -0.006(2) 0.040(2) C5B 0.047(2) -0.013(2) 0.005(2) 0.041(2) 0.003(2) 0.031(2) C6B 0.054(2) -0.011(2) -0.006(2) 0.030(2) 0.005(2) 0.062(3) C1C 0.037(2) 0.0007(13) 0.0035(13) 0.026(2) -0.0044(13) 0.024(2) C2C 0.035(2) 0.0054(14) -0.002(2) 0.028(2) -0.005(2) 0.044(2) C3C 0.028(2) -0.0027(13) 0.0042(12) 0.034(2) 0.0063(13) 0.025(2) C4C 0.041(2) -0.0057(14) 0.002(2) 0.026(2) 0.0054(14) 0.041(2) C5C 0.029(2) 0.0032(13) -0.0020(13) 0.037(2) 0.0023(13) 0.023(2) C6C 0.025(2) -0.0007(13) 0.0005(14) 0.034(2) 0.002(2) 0.041(2) C1D 0.046(2) -0.001(2) 0.001(2) 0.031(2) -0.0044(14) 0.028(2) C2D 0.044(2) 0.009(2) -0.005(2) 0.028(2) -0.006(2) 0.050(2) C3D 0.037(2) -0.002(2) 0.0087(14) 0.037(2) 0.0045(14) 0.028(2) C4D 0.046(2) -0.009(2) 0.009(2) 0.029(2) 0.002(2) 0.049(2) C5D 0.038(2) 0.005(2) -0.0056(14) 0.041(2) 0.003(2) 0.027(2) C6D 0.028(2) -0.006(2) -0.004(2) 0.042(2) 0.002(2) 0.055(2) _cod_database_code 2003229