#------------------------------------------------------------------------------ #$Date: 2017-10-13 01:48:21 +0100 (Fri, 13 Oct 2017) $ #$Revision: 201957 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/21/2012136.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_2012136 loop_ _publ_author_name 'Dubberley, Stuart R.' 'Tyrrell, Ben R.' 'Mountford, Philip' _publ_section_title ; Tetrakis(dimethylamido)vanadium(IV) ; _journal_issue 8 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first 902 _journal_page_last 904 _journal_paper_doi 10.1107/S0108270101008368 _journal_volume 57 _journal_year 2001 _chemical_formula_moiety ' C8 H24 N4 V1 ' _chemical_formula_sum 'C8 H24 N4 V' _chemical_formula_weight 227.25 _chemical_name_systematic ; Tetrakis(dimethylamido)vanadium ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _cell_angle_alpha 75.6616(10) _cell_angle_beta 79.4036(11) _cell_angle_gamma 84.9664(9) _cell_formula_units_Z 4 _cell_length_a 8.2903(2) _cell_length_b 12.0158(2) _cell_length_c 13.8350(3) _cell_measurement_reflns_used 5348 _cell_measurement_temperature 150 _cell_measurement_theta_max 27.49 _cell_measurement_theta_min 1.00 _cell_volume 1311.18(5) _computing_cell_refinement DENZO _computing_data_collection 'Kappa-CCD software COLLECT (Nonius, 2000)' _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, Prout & Pearce et al., 1996)' _computing_publication_material CRYSTALS _computing_structure_refinement 'CRYSTALS (Watkin, Prout et al., 1996)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_ambient_temperature 150 _diffrn_measured_fraction_theta_full .98 _diffrn_measured_fraction_theta_max .98 _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method CCD _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .02 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 10654 _diffrn_reflns_theta_full 27.49 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_min 1.00 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu .73 _exptl_absorpt_correction_T_max .864 _exptl_absorpt_correction_T_min .864 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(DENZO; Otwinowski & Minor, 1997)' _exptl_crystal_colour 'dark green' _exptl_crystal_density_diffrn 1.151 _exptl_crystal_density_meas ? _exptl_crystal_density_method none _exptl_crystal_description block _exptl_crystal_F_000 492 _exptl_crystal_size_max .30 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .20 _refine_diff_density_max .71 _refine_diff_density_min -.83 _refine_ls_extinction_coef none _refine_ls_goodness_of_fit_ref 1.05 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 427 _refine_ls_number_reflns 5883 _refine_ls_number_restraints 0 _refine_ls_R_factor_gt .0325 _refine_ls_shift/su_max .006 _refine_ls_structure_factor_coef F _refine_ls_weighting_details ; Chebychev polynomial with 5 parameters, (Carruthers & Watkin, 1979), 0.895 0.532 0.456 -.541E-01 -.147 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_ref .0431 _reflns_number_gt 4773 _reflns_number_total 5886 _reflns_threshold_expression I>2\s(I) _cod_data_source_file gg1056.cif _cod_data_source_block I _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic ' changed to 'triclinic' 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 The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic ' changed to 'triclinic' 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_values 1715 2011-07-08 13:25:40Z adriana The following automatic conversions were performed: '_exptl_crystal_density_meas' value 'not measured' was changed to '?' - the value is perceived as not measured. Automatic conversion script Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas ; _cod_original_sg_symbol_H-M 'P -1 ' _cod_original_formula_sum 'C8 H24 N4 V1' _cod_database_code 2012136 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z 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_occupancy V1 .22069(3) .248426(19) -.473572(17) .0206 Uani 1.0000 N1 .34951(15) .36961(11) -.55220(10) .0261 Uani 1.0000 N2 .36549(15) .13317(11) -.41670(10) .0267 Uani 1.0000 N3 .07447(15) .30263(11) -.37399(9) .0266 Uani 1.0000 N4 .09240(15) .18648(11) -.54380(10) .0254 Uani 1.0000 C1 .2858(2) .48730(15) -.58253(14) .0364 Uani 1.0000 C2 .5100(2) .35317(17) -.61184(13) .0344 Uani 1.0000 C3 .5067(2) .15807(15) -.37819(14) .0329 Uani 1.0000 C4 .3247(2) .01340(15) -.37757(16) .0386 Uani 1.0000 C5 .1192(2) .38497(16) -.32295(13) .0348 Uani 1.0000 C6 -.0607(2) .23496(17) -.31178(14) .0360 Uani 1.0000 C7 -.06547(19) .23800(16) -.56632(13) .0316 Uani 1.0000 C8 .1552(2) .10298(15) -.60336(13) .0308 Uani 1.0000 H11 .180(3) .496(2) -.5433(18) .044(6) Uiso 1.0000 H12 .278(3) .5101(19) -.6558(17) .037(5) Uiso 1.0000 H13 .360(3) .539(2) -.5697(19) .053(7) Uiso 1.0000 H21 .508(3) .3714(19) -.6859(17) .037(5) Uiso 1.0000 H22 .547(3) .273(2) -.594(2) .052(7) Uiso 1.0000 H23 .596(3) .396(2) -.599(2) .055(7) Uiso 1.0000 H31 .491(3) .132(2) -.301(2) .055(7) Uiso 1.0000 H32 .610(3) .115(2) -.4042(19) .049(6) Uiso 1.0000 H33 .529(3) .238(2) -.4011(17) .044(6) Uiso 1.0000 H41 .232(3) .000(2) -.3986(18) .043(6) Uiso 1.0000 H42 .311(3) -.008(2) -.304(2) .055(7) Uiso 1.0000 H43 .408(3) -.038(2) -.402(2) .059(7) Uiso 1.0000 H51 .210(3) .427(2) -.3627(19) .049(6) Uiso 1.0000 H52 .151(3) .348(2) -.256(2) .051(6) Uiso 1.0000 H53 .026(3) .444(2) -.3121(18) .048(6) Uiso 1.0000 H61 -.158(3) .284(2) -.296(2) .055(7) Uiso 1.0000 H62 -.036(3) .195(2) -.246(2) .052(6) Uiso 1.0000 H63 -.098(3) .183(2) -.346(2) .054(7) Uiso 1.0000 H71 -.108(3) .291(2) -.5275(17) .037(5) Uiso 1.0000 H72 -.148(3) .182(2) -.5511(19) .050(6) Uiso 1.0000 H73 -.059(3) .280(2) -.636(2) .052(7) Uiso 1.0000 H81 .165(3) .138(2) -.678(2) .050(6) Uiso 1.0000 H82 .262(3) .0739(19) -.5909(16) .036(5) Uiso 1.0000 H83 .089(3) .039(2) -.5861(17) .045(6) Uiso 1.0000 V1A .20452(3) .247431(19) .023480(17) .0198 Uani 1.0000 N1A .28403(15) .27243(11) .13365(9) .0251 Uani 1.0000 N2A -.02305(14) .27234(11) .04767(9) .0238 Uani 1.0000 N3A .26320(16) .09759(11) .00992(11) .0289 Uani 1.0000 N4A .29526(15) .34829(11) -.09637(9) .0253 Uani 1.0000 C1A .2228(2) .36610(15) .18210(13) .0310 Uani 1.0000 C2A .4500(2) .23409(17) .15061(15) .0368 Uani 1.0000 C3A -.1259(2) .30240(15) -.03036(12) .0292 Uani 1.0000 C4A -.11677(19) .22405(14) .14691(12) .0285 Uani 1.0000 C5A .2706(3) -.00061(16) .09426(18) .0443 Uani 1.0000 C6A .2459(2) .06276(17) -.08104(16) .0394 Uani 1.0000 C7A .2451(2) .46969(14) -.11801(13) .0318 Uani 1.0000 C8A .4560(2) .32859(17) -.15403(14) .0350 Uani 1.0000 H11A .217(3) .341(2) .2577(18) .041(6) Uiso 1.0000 H12A .116(3) .393(2) .1693(17) .041(6) Uiso 1.0000 H13A .287(3) .430(2) .1590(18) .044(6) Uiso 1.0000 H21A .526(3) .301(2) .126(2) .059(7) Uiso 1.0000 H22A .496(3) .177(2) .1162(19) .048(6) Uiso 1.0000 H23A .447(3) .204(2) .224(2) .050(6) Uiso 1.0000 H31A -.210(3) .361(2) -.0175(17) .042(6) Uiso 1.0000 H32A -.059(3) .333(2) -.0935(18) .043(6) Uiso 1.0000 H33A -.187(3) .233(2) -.0333(18) .049(6) Uiso 1.0000 H41A -.187(3) .161(2) .1499(17) .040(5) Uiso 1.0000 H42A -.050(3) .200(2) .1970(19) .044(6) Uiso 1.0000 H43A -.193(3) .281(2) .1718(17) .041(6) Uiso 1.0000 H51A .357(4) -.055(3) .083(2) .063(8) Uiso 1.0000 H52A .285(3) .020(2) .151(2) .054(7) Uiso 1.0000 H53A .184(4) -.043(3) .105(2) .070(8) Uiso 1.0000 H61A .143(3) .022(2) -.0730(18) .048(6) Uiso 1.0000 H62A .244(3) .130(2) -.137(2) .050(6) Uiso 1.0000 H63A .342(3) .016(2) -.104(2) .057(7) Uiso 1.0000 H71A .140(3) .482(2) -.0799(19) .050(6) Uiso 1.0000 H72A .325(3) .510(2) -.1031(19) .049(6) Uiso 1.0000 H73A .237(3) .4982(19) -.1882(18) .038(5) Uiso 1.0000 H81A .488(3) .253(2) -.1345(19) .048(6) Uiso 1.0000 H82A .455(3) .351(2) -.2251(19) .047(6) Uiso 1.0000 H83A .539(4) .368(2) -.139(2) .060(7) Uiso 1.0000 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 .02026(12) .02027(13) .02093(13) -.00315(9) -.00304(9) -.00368(9) N1 .0253(6) .0245(6) .0271(6) -.0052(5) -.0035(5) -.0025(5) N2 .0255(6) .0230(6) .0315(6) -.0025(5) -.0076(5) -.0035(5) N3 .0266(6) .0293(6) .0241(6) -.0039(5) -.0024(5) -.0072(5) N4 .0227(6) .0267(6) .0282(6) -.0021(5) -.0048(5) -.0084(5) C1 .0450(10) .0246(8) .0353(9) -.0031(7) -.0046(7) -.0006(6) C2 .0271(7) .0402(9) .0334(8) -.0103(7) .0002(6) -.0050(7) C3 .0290(8) .0324(8) .0392(9) -.0007(6) -.0129(6) -.0071(7) C4 .0417(9) .0263(8) .0460(10) -.0065(7) -.0152(8) .0027(7) C5 .0409(9) .0376(9) .0298(8) -.0046(7) -.0063(7) -.0139(7) C6 .0338(8) .0396(9) .0306(8) -.0084(7) .0054(6) -.0064(7) C7 .0250(7) .0383(9) .0344(8) -.0003(6) -.0077(6) -.0125(7) C8 .0326(8) .0307(8) .0316(8) -.0019(6) -.0049(6) -.0122(7) V1A .01867(12) .01888(12) .02131(13) -.00163(8) -.00251(9) -.00414(9) N1A .0202(5) .0285(6) .0268(6) -.0014(5) -.0058(4) -.0057(5) N2A .0217(5) .0258(6) .0242(6) -.0013(4) -.0050(4) -.0057(5) N3A .0292(6) .0205(6) .0364(7) -.0005(5) -.0044(5) -.0066(5) N4A .0272(6) .0240(6) .0240(6) -.0031(5) -.0019(5) -.0055(5) C1A .0324(8) .0303(8) .0327(8) -.0020(6) -.0086(6) -.0096(6) C2A .0221(7) .0460(10) .0440(10) -.0009(7) -.0099(7) -.0115(8) C3A .0257(7) .0356(8) .0296(8) .0017(6) -.0090(6) -.0117(6) C4A .0228(7) .0335(8) .0277(7) -.0039(6) -.0027(6) -.0047(6) C5A .0492(11) .0239(8) .0548(12) -.0043(8) -.0110(9) .0025(8) C6A .0393(9) .0312(9) .0528(11) -.0018(7) -.0074(8) -.0197(8) C7A .0402(9) .0221(7) .0320(8) -.0049(6) -.0035(7) -.0048(6) C8A .0291(8) .0361(9) .0355(9) -.0051(7) .0034(6) -.0053(7) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C ' .0020 .0020 International_Tables_Vol_IV_Table_2.2B 'H ' .0000 .0000 International_Tables_Vol_IV_Table_2.2B 'N ' .0040 .0030 International_Tables_Vol_IV_Table_2.2B 'V ' .2670 .5300 International_Tables_Vol_IV_Table_2.2B loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag N1 V1 N2 106.53(6) yes N1 V1 N3 108.41(6) yes N2 V1 N3 111.42(6) yes N1 V1 N4 115.28(6) yes N2 V1 N4 109.00(6) yes N3 V1 N4 106.26(5) yes V1 N1 C1 123.67(11) yes V1 N1 C2 123.62(11) yes C1 N1 C2 110.81(14) no V1 N2 C3 122.50(10) yes V1 N2 C4 123.70(11) yes C3 N2 C4 111.12(13) no V1 N3 C5 122.77(11) yes V1 N3 C6 121.60(11) yes C5 N3 C6 110.85(13) no V1 N4 C7 122.60(10) yes V1 N4 C8 123.80(10) yes C7 N4 C8 111.74(12) no N1 C1 H11 109.4(14) no N1 C1 H12 112.3(13) no H11 C1 H12 109.3(19) no N1 C1 H13 109.0(15) no H11 C1 H13 109(2) no H12 C1 H13 108.0(19) no N1 C2 H21 112.8(13) no N1 C2 H22 110.0(15) no H21 C2 H22 105(2) no N1 C2 H23 113.6(15) no H21 C2 H23 109.4(19) no H22 C2 H23 105(2) no N2 C3 H31 111.3(14) no N2 C3 H32 111.4(14) no H31 C3 H32 106(2) no N2 C3 H33 110.7(14) no H31 C3 H33 111(2) no H32 C3 H33 105.8(19) no N2 C4 H41 110.5(15) no N2 C4 H42 111.5(16) no H41 C4 H42 110(2) no N2 C4 H43 112.5(16) no H41 C4 H43 105(2) no H42 C4 H43 107(2) no N3 C5 H51 110.5(15) no N3 C5 H52 113.2(15) no H51 C5 H52 107(2) no N3 C5 H53 111.4(14) no H51 C5 H53 107(2) no H52 C5 H53 108(2) no N3 C6 H61 111.3(16) no N3 C6 H62 112.4(15) no H61 C6 H62 104(2) no N3 C6 H63 112.4(15) no H61 C6 H63 105(2) no H62 C6 H63 112(2) no N4 C7 H71 112.6(14) no N4 C7 H72 111.9(15) no H71 C7 H72 105(2) no N4 C7 H73 112.2(15) no H71 C7 H73 106(2) no H72 C7 H73 109(2) no N4 C8 H81 112.0(14) no N4 C8 H82 110.5(13) no H81 C8 H82 106.8(19) no N4 C8 H83 111.7(14) no H81 C8 H83 109(2) no H82 C8 H83 106.3(19) no N1A V1A N2A 107.16(5) yes N1A V1A N3A 109.74(6) yes N2A V1A N3A 111.48(6) yes N1A V1A N4A 110.73(5) yes N2A V1A N4A 110.03(6) yes N3A V1A N4A 107.73(6) yes V1A N1A C1A 123.30(10) yes V1A N1A C2A 120.92(11) yes C1A N1A C2A 111.22(13) no V1A N2A C3A 124.70(10) yes V1A N2A C4A 120.00(10) yes C3A N2A C4A 112.02(12) no V1A N3A C5A 124.03(13) yes V1A N3A C6A 120.92(11) yes C5A N3A C6A 111.45(15) no V1A N4A C7A 121.02(11) yes V1A N4A C8A 123.65(11) yes C7A N4A C8A 111.20(13) no N1A C1A H11A 111.5(13) no N1A C1A H12A 111.4(14) no H11A C1A H12A 107.5(19) no N1A C1A H13A 113.2(15) no H11A C1A H13A 107.4(19) no H12A C1A H13A 105(2) no N1A C2A H21A 110.6(16) no N1A C2A H22A 113.4(15) no H21A C2A H22A 106(2) no N1A C2A H23A 108.0(15) no H21A C2A H23A 109(2) no H22A C2A H23A 110(2) no N2A C3A H31A 111.5(14) no N2A C3A H32A 108.8(14) no H31A C3A H32A 107.3(19) no N2A C3A H33A 111.5(14) no H31A C3A H33A 106.3(19) no H32A C3A H33A 111(2) no N2A C4A H41A 115.3(13) no N2A C4A H42A 112.6(14) no H41A C4A H42A 109(2) no N2A C4A H43A 111.7(13) no H41A C4A H43A 104.1(18) no H42A C4A H43A 103.2(19) no N3A C5A H51A 114.5(17) no N3A C5A H52A 111.9(17) no H51A C5A H52A 105(2) no N3A C5A H53A 111(2) no H51A C5A H53A 101(3) no H52A C5A H53A 113(3) no N3A C6A H61A 112.8(14) no N3A C6A H62A 110.0(15) no H61A C6A H62A 108(2) no N3A C6A H63A 111.3(16) no H61A C6A H63A 111(2) no H62A C6A H63A 104(2) no N4A C7A H71A 110.5(16) no N4A C7A H72A 108.1(16) no H71A C7A H72A 112(2) no N4A C7A H73A 110.9(13) no H71A C7A H73A 107(2) no H72A C7A H73A 108(2) no N4A C8A H81A 109.0(16) no N4A C8A H82A 111.2(15) no H81A C8A H82A 111(2) no N4A C8A H83A 112.5(17) no H81A C8A H83A 104(2) no H82A C8A H83A 109(2) no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag V1 N1 . . 1.8721(12) yes V1 N2 . . 1.8692(13) yes V1 N3 . . 1.8664(13) yes V1 N4 . . 1.8721(12) yes N1 C1 . . 1.453(2) no N1 C2 . . 1.456(2) no N2 C3 . . 1.4536(19) no N2 C4 . . 1.453(2) no N3 C5 . . 1.457(2) no N3 C6 . . 1.455(2) no N4 C7 . . 1.4512(19) no N4 C8 . . 1.455(2) no C1 H11 . . .96(3) no C1 H12 . . 1.00(2) no C1 H13 . . .98(3) no C2 H21 . . 1.00(2) no C2 H22 . . .97(3) no C2 H23 . . .98(3) no C3 H31 . . 1.02(3) no C3 H32 . . 1.01(3) no C3 H33 . . .96(2) no C4 H41 . . .91(3) no C4 H42 . . .98(3) no C4 H43 . . .96(3) no C5 H51 . . .95(3) no C5 H52 . . .99(3) no C5 H53 . . 1.02(3) no C6 H61 . . .98(3) no C6 H62 . . .97(3) no C6 H63 . . .97(3) no C7 H71 . . .94(2) no C7 H72 . . .96(3) no C7 H73 . . .96(3) no C8 H81 . . 1.00(3) no C8 H82 . . .96(2) no C8 H83 . . .94(2) no V1A N1A . . 1.8652(12) yes V1A N2A . . 1.8653(12) yes V1A N3A . . 1.8691(13) yes V1A N4A . . 1.8681(13) yes N1A C1A . . 1.457(2) yes N1A C2A . . 1.4539(19) no N2A C3A . . 1.4541(19) no N2A C4A . . 1.4552(19) no N3A C5A . . 1.446(2) no N3A C6A . . 1.455(2) no N4A C7A . . 1.454(2) no N4A C8A . . 1.454(2) no C1A H11A . . 1.01(2) no C1A H12A . . .94(2) no C1A H13A . . .93(2) no C2A H21A . . 1.01(3) no C2A H22A . . .94(3) no C2A H23A . . .98(3) no C3A H31A . . .97(2) no C3A H32A . . .95(2) no C3A H33A . . 1.02(2) no C4A H41A . . .98(2) no C4A H42A . . .94(3) no C4A H43A . . .98(2) no C5A H51A . . .94(3) no C5A H52A . . .91(3) no C5A H53A . . .89(3) no C6A H61A . . 1.00(2) no C6A H62A . . .97(3) no C6A H63A . . .98(3) no C7A H71A . . .95(3) no C7A H72A . . .94(3) no C7A H73A . . .96(2) no C8A H81A . . .92(3) no C8A H82A . . .96(3) no C8A H83A . . .94(3) no loop_ _cod_related_entry_id _cod_related_entry_database _cod_related_entry_code 1 ChemSpider 24724297