#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/24/2012498.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_2012498 loop_ _publ_author_name 'Mach, Karel' 'Kubi\O,O':2(\h^5^)-Cyclopentadienylcarboxylato][2(\h^5^)-diphenylphosphinocyclopentadienyl]bis[1,1(\h^5^)-tetramethylcyclopentadienyl]iron(II)titanium(III)' _journal_issue 2 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m116 _journal_page_last m118 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[Fe Ti (C9 H13)2 (C6 H4 O2) (C17 H14 P)]' _chemical_formula_moiety 'C41 H44 Fe O2 P Ti' _chemical_formula_sum 'C41 H44 Fe O2 P Ti' _chemical_formula_weight 703.48 _chemical_name_systematic ; \m-1\k^2^O,O':2(\h^5^)-Cyclopentadienylcarboxylato- 2(\h^5^)-diphenylphosphinocyclopentadienyl-bis[1,1(\h^5^)- tetramethylcyclopentadienyl]iron(II)titanium(III) ; _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' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 97.3941(5) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.46600(10) _cell_length_b 29.5260(3) _cell_length_c 14.10020(10) _cell_measurement_reflns_used 97200 _cell_measurement_temperature 150 _cell_measurement_theta_max 27.5 _cell_measurement_theta_min 1.0 _cell_volume 3495.28(6) _computing_cell_refinement 'HKL SCALEPACK (Otwinowski & Minor 1997)' _computing_data_collection 'COLLECT (Nonius, 1997-2000)' _computing_data_reduction 'HKL DENZO (Otwinowski & Minor 1997) and SCALEPACK' _computing_molecular_graphics 'PLATON (Spek, 1999)' _computing_publication_material 'SHELXL97 and PLATON' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _diffrn_ambient_temperature 150 _diffrn_detector_area_resol_mean .110 _diffrn_measured_fraction_theta_full .995 _diffrn_measured_fraction_theta_max .995 _diffrn_measurement_device_type 'Nonius KappaCCD area-detector' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .049 _diffrn_reflns_av_sigmaI/netI .029 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_k_min -38 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 47188 _diffrn_reflns_theta_full 27.49 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_min 2.99 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu .724 _exptl_absorpt_correction_T_max .757 _exptl_absorpt_correction_T_min .606 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(SORTAV; Blessing, 1997)' _exptl_crystal_colour 'dark red-brown' _exptl_crystal_density_diffrn 1.337 _exptl_crystal_density_meas 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 1476 _exptl_crystal_size_max .75 _exptl_crystal_size_mid .50 _exptl_crystal_size_min .40 _refine_diff_density_max .29 _refine_diff_density_min -.34 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 415 _refine_ls_number_reflns 7976 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all .040 _refine_ls_R_factor_gt .033 _refine_ls_shift/su_max .001 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0368P)^2^+1.8480P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .082 _refine_ls_wR_factor_ref .085 _reflns_number_gt 6981 _reflns_number_total 7976 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file gd1183.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_database_code 2012498 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 Fe .57108(3) .204214(7) .239415(16) .02484(7) Uani d . 1 . . Fe Ti .95668(3) .050262(10) .247736(19) .02378(8) Uani d . 1 . . Ti P .24225(5) .273465(14) .21997(3) .02787(10) Uani d . 1 . . P O1 .95754(13) .12333(4) .24404(8) .0283(2) Uani d . 1 . . O O2 .73241(13) .08608(4) .21874(8) .0264(2) Uani d . 1 . . O C1 .72893(19) .16481(5) .17876(11) .0267(3) Uani d . 1 . . C C2 .7902(2) .20966(6) .19218(13) .0314(4) Uani d . 1 . . C H2 .8856 .2178 .2285 .038 Uiso calc R 1 . . H C3 .6805(2) .23970(6) .14057(13) .0372(4) Uani d . 1 . . C H3 .6911 .2710 .1374 .045 Uiso calc R 1 . . H C4 .5515(2) .21382(6) .09454(13) .0359(4) Uani d . 1 . . C H4 .4634 .2252 .0557 .043 Uiso calc R 1 . . H C5 .5800(2) .16741(6) .11812(12) .0312(4) Uani d . 1 . . C H5 .5139 .1432 .0978 .037 Uiso calc R 1 . . H C6 .38382(19) .23626(5) .28874(12) .0273(3) Uani d . 1 . . C C7 .3654(2) .18802(6) .29243(12) .0307(3) Uani d . 1 . . C H7 .2811 .1714 .2609 .037 Uiso calc R 1 . . H C8 .4981(2) .16998(6) .35243(12) .0325(4) Uani d . 1 . . C H8 .5154 .1395 .3672 .039 Uiso calc R 1 . . H C9 .5998(2) .20641(6) .38603(12) .0315(4) Uani d . 1 . . C H9 .6955 .2040 .4262 .038 Uiso calc R 1 . . H C10 .5298(2) .24711(6) .34747(12) .0288(3) Uani d . 1 . . C H10 .5717 .2760 .3585 .035 Uiso calc R 1 . . H C11 .80852(19) .12306(5) .21718(11) .0255(3) Uani d . 1 . . C C12 .36132(19) .32536(6) .21845(13) .0313(4) Uani d . 1 . . C C13 .4242(2) .33569(7) .13431(15) .0401(4) Uani d . 1 . . C H13 .3999 .3173 .0809 .048 Uiso calc R 1 . . H C14 .5220(3) .37288(8) .12909(18) .0519(6) Uani d . 1 . . C H14 .5646 .3789 .0728 .062 Uiso calc R 1 . . H C15 .5563(2) .40090(7) .2066(2) .0548(6) Uani d . 1 . . C H15 .6222 .4259 .2029 .066 Uiso calc R 1 . . H C16 .4929(2) .39200(7) .29052(18) .0484(5) Uani d . 1 . . C H16 .5151 .4112 .3427 .058 Uiso calc R 1 . . H C17 .3958(2) .35424(6) .29683(14) .0365(4) Uani d . 1 . . C H17 .3540 .3483 .3534 .044 Uiso calc R 1 . . H C18 .11076(19) .28714(6) .30973(12) .0280(3) Uani d . 1 . . C C19 -.0129(2) .31774(6) .28428(14) .0353(4) Uani d . 1 . . C H19 -.0212 .3322 .2252 .042 Uiso calc R 1 . . H C20 -.1239(2) .32684(7) .34622(15) .0419(4) Uani d . 1 . . C H20 -.2050 .3476 .3287 .050 Uiso calc R 1 . . H C21 -.1147(2) .30530(7) .43359(14) .0392(4) Uani d . 1 . . C H21 -.1899 .3112 .4746 .047 Uiso calc R 1 . . H C22 .0070(2) .27491(7) .45975(14) .0394(4) Uani d . 1 . . C H22 .0141 .2604 .5187 .047 Uiso calc R 1 . . H C23 .1191(2) .26594(6) .39823(13) .0353(4) Uani d . 1 . . C H23 .2007 .2454 .4166 .042 Uiso calc R 1 . . H C30 1.1007(2) .00824(6) .37137(11) .0299(3) Uani d . 1 . . C H30 1.1903 -.0078 .3590 .036 Uiso calc R 1 . . H C31 1.10027(19) .05370(6) .40117(11) .0290(3) Uani d . 1 . . C C32 .9399(2) .06473(6) .41159(11) .0301(3) Uani d . 1 . . C C33 .8447(2) .02570(6) .38837(12) .0317(4) Uani d . 1 . . C C34 .9437(2) -.00937(6) .36313(12) .0316(4) Uani d . 1 . . C C35 1.2422(2) .08408(7) .42014(14) .0399(4) Uani d . 1 . . C H35A 1.2736 .0864 .4879 .048 Uiso calc R 1 . . H H35B 1.2157 .1136 .3944 .048 Uiso calc R 1 . . H H35C 1.3285 .0718 .3903 .048 Uiso calc R 1 . . H C36 .8814(2) .10879(7) .44673(13) .0422(4) Uani d . 1 . . C H36A .7854 .1176 .4072 .051 Uiso calc R 1 . . H H36B .9612 .1317 .4439 .051 Uiso calc R 1 . . H H36C .8602 .1053 .5116 .051 Uiso calc R 1 . . H C37 .6686(2) .02262(8) .39332(14) .0458(5) Uani d . 1 . . C H37A .6281 -.0051 .3642 .055 Uiso calc R 1 . . H H37B .6156 .0478 .3599 .055 Uiso calc R 1 . . H H37C .6496 .0232 .4590 .055 Uiso calc R 1 . . H C38 .8952(3) -.05746(7) .34001(14) .0444(5) Uani d . 1 . . C H38A .8926 -.0741 .3983 .053 Uiso calc R 1 . . H H38B .9706 -.0712 .3035 .053 Uiso calc R 1 . . H H38C .7914 -.0578 .3035 .053 Uiso calc R 1 . . H C40 1.0551(2) -.00696(6) .15835(12) .0310(4) Uani d . 1 . . C H40 1.0843 -.0343 .1882 .037 Uiso calc R 1 . . H C41 1.1577(2) .03072(6) .15180(12) .0313(4) Uani d . 1 . . C C42 1.0674(2) .06464(6) .09884(11) .0303(3) Uani d . 1 . . C C43 .9105(2) .04824(6) .07489(11) .0284(3) Uani d . 1 . . C C44 .9014(2) .00394(6) .11205(11) .0294(3) Uani d . 1 . . C C45 1.3338(2) .03217(8) .18530(14) .0438(5) Uani d . 1 . . C H45A 1.3915 .0257 .1326 .053 Uiso calc R 1 . . H H45B 1.3598 .0100 .2346 .053 Uiso calc R 1 . . H H45C 1.3624 .0617 .2101 .053 Uiso calc R 1 . . H C46 1.1289(2) .10963(7) .07051(13) .0391(4) Uani d . 1 . . C H46A 1.1251 .1109 .0022 .047 Uiso calc R 1 . . H H46B 1.2369 .1134 .0997 .047 Uiso calc R 1 . . H H46C 1.0640 .1334 .0914 .047 Uiso calc R 1 . . H C47 .7770(2) .07199(6) .01381(12) .0361(4) Uani d . 1 . . C H47A .7741 .0623 -.0514 .043 Uiso calc R 1 . . H H47B .7940 .1041 .0175 .043 Uiso calc R 1 . . H H47C .6777 .0648 .0363 .043 Uiso calc R 1 . . H C48 .7570(2) -.02593(7) .09934(13) .0390(4) Uani d . 1 . . C H48A .6735 -.0121 .1294 .047 Uiso calc R 1 . . H H48B .7831 -.0549 .1282 .047 Uiso calc R 1 . . H H48C .7219 -.0299 .0324 .047 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 Fe .02460(12) .02365(12) .02713(12) .00319(8) .00659(9) -.00018(9) Ti .02200(14) .02672(15) .02231(14) .00377(10) .00171(10) .00053(11) P .0247(2) .0295(2) .0292(2) .00203(16) .00268(16) -.00304(17) O1 .0243(6) .0290(6) .0315(6) .0020(4) .0028(5) -.0015(5) O2 .0236(5) .0271(6) .0283(6) .0025(4) .0031(4) .0002(4) C1 .0266(8) .0284(8) .0264(8) .0049(6) .0087(6) -.0005(6) C2 .0277(8) .0300(8) .0385(9) .0013(6) .0122(7) .0020(7) C3 .0425(10) .0307(9) .0420(10) .0065(7) .0201(8) .0091(8) C4 .0393(10) .0416(10) .0284(8) .0145(8) .0101(7) .0069(7) C5 .0310(9) .0361(9) .0269(8) .0069(7) .0047(7) -.0036(7) C6 .0248(8) .0285(8) .0297(8) .0025(6) .0080(6) -.0034(6) C7 .0285(8) .0293(8) .0358(9) -.0014(7) .0100(7) -.0026(7) C8 .0352(9) .0306(9) .0337(9) .0044(7) .0125(7) .0057(7) C9 .0300(9) .0377(9) .0273(8) .0064(7) .0055(7) -.0003(7) C10 .0281(8) .0292(8) .0292(8) .0033(6) .0043(6) -.0056(7) C11 .0267(8) .0284(8) .0222(7) .0028(6) .0064(6) -.0025(6) C12 .0247(8) .0285(8) .0403(9) .0061(6) .0022(7) .0039(7) C13 .0350(10) .0412(10) .0442(10) .0068(8) .0053(8) .0107(8) C14 .0398(11) .0486(12) .0681(15) .0041(9) .0093(10) .0269(11) C15 .0313(10) .0357(11) .0952(19) .0015(8) .0004(11) .0234(12) C16 .0323(10) .0312(10) .0776(15) .0054(8) -.0091(10) -.0073(10) C17 .0280(9) .0321(9) .0483(11) .0050(7) .0007(8) -.0034(8) C18 .0225(8) .0288(8) .0325(8) -.0003(6) .0023(6) -.0046(7) C19 .0288(9) .0359(9) .0409(10) .0055(7) .0033(7) .0023(8) C20 .0274(9) .0416(10) .0567(12) .0092(7) .0053(8) -.0052(9) C21 .0281(9) .0446(10) .0463(11) -.0007(8) .0108(8) -.0115(9) C22 .0372(10) .0471(11) .0349(9) .0034(8) .0081(8) -.0028(8) C23 .0287(9) .0415(10) .0356(9) .0071(7) .0031(7) .0001(8) C30 .0284(8) .0360(9) .0247(8) .0065(7) .0006(6) .0049(7) C31 .0257(8) .0375(9) .0229(7) .0011(7) -.0006(6) .0019(7) C32 .0274(8) .0401(9) .0223(7) .0057(7) .0014(6) .0013(7) C33 .0258(8) .0456(10) .0231(8) -.0014(7) .0007(6) .0070(7) C34 .0340(9) .0363(9) .0231(8) -.0013(7) -.0015(7) .0060(7) C35 .0317(9) .0497(11) .0370(10) -.0077(8) -.0003(8) -.0004(8) C36 .0445(11) .0519(12) .0301(9) .0147(9) .0042(8) -.0041(8) C37 .0275(9) .0709(14) .0389(10) -.0023(9) .0039(8) .0127(10) C38 .0575(13) .0387(10) .0349(10) -.0095(9) -.0018(9) .0076(8) C40 .0359(9) .0317(8) .0258(8) .0106(7) .0056(7) .0009(7) C41 .0272(8) .0409(10) .0264(8) .0075(7) .0056(6) .0003(7) C42 .0323(9) .0354(9) .0239(8) .0053(7) .0064(6) .0005(7) C43 .0301(8) .0333(9) .0218(7) .0078(7) .0038(6) -.0019(6) C44 .0319(9) .0321(8) .0244(8) .0039(7) .0045(6) -.0046(6) C45 .0283(9) .0670(14) .0362(10) .0090(9) .0050(8) .0041(9) C46 .0411(10) .0424(10) .0349(9) -.0012(8) .0086(8) .0043(8) C47 .0384(10) .0434(10) .0254(8) .0126(8) -.0004(7) -.0021(7) C48 .0417(10) .0404(10) .0344(9) -.0040(8) .0027(8) -.0064(8) 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 Fe C1 . 2.0409(15) yes Fe C2 . 2.0566(17) yes Fe C3 . 2.0569(17) yes Fe C4 . 2.0478(17) yes Fe C5 . 2.0360(17) yes Fe C6 . 2.0435(16) yes Fe C7 . 2.0380(17) yes Fe C8 . 2.0484(17) yes Fe C9 . 2.0512(17) yes Fe C10 . 2.0457(16) yes Ti O1 . 2.1582(12) yes Ti O2 . 2.1658(11) yes Ti C30 . 2.3489(16) yes Ti C31 . 2.3435(16) yes Ti C32 . 2.3718(16) yes Ti C33 . 2.4166(16) yes Ti C34 . 2.4095(17) yes Ti C40 . 2.3256(16) yes Ti C41 . 2.3771(16) yes Ti C42 . 2.4440(16) yes Ti C43 . 2.4189(16) yes Ti C44 . 2.3493(16) yes P C6 . 1.8122(17) yes P C12 . 1.8359(18) yes P C18 . 1.8349(17) yes O1 C11 . 1.2697(19) yes O2 C11 . 1.2693(19) yes C1 C2 . 1.426(2) no C1 C5 . 1.431(2) no C1 C11 . 1.474(2) yes C2 C3 . 1.416(3) no C2 H2 . .9300 no C3 C4 . 1.420(3) no C3 H3 . .9300 no C4 C5 . 1.423(2) no C4 H4 . .9300 no C5 H5 . .9300 no C6 C10 . 1.433(2) no C6 C7 . 1.434(2) no C7 C8 . 1.420(3) no C7 H7 . .9300 no C8 C9 . 1.421(3) no C8 H8 . .9300 no C9 C10 . 1.417(2) no C9 H9 . .9300 no C10 H10 . .9300 no C12 C13 . 1.395(3) no C12 C17 . 1.397(3) no C13 C14 . 1.383(3) no C13 H13 . .9300 no C14 C15 . 1.372(4) no C14 H14 . .9300 no C15 C16 . 1.386(3) no C15 H15 . .9300 no C16 C17 . 1.394(3) no C16 H16 . .9300 no C17 H17 . .9300 no C18 C23 . 1.390(2) no C18 C19 . 1.395(2) no C19 C20 . 1.389(3) no C19 H19 . .9300 no C20 C21 . 1.380(3) no C20 H20 . .9300 no C21 C22 . 1.380(3) no C21 H21 . .9300 no C22 C23 . 1.391(3) no C22 H22 . .9300 no C23 H23 . .9300 no C30 C31 . 1.407(2) no C30 C34 . 1.418(2) no C30 H30 . .9300 no C31 C32 . 1.422(2) no C31 C35 . 1.496(2) no C32 C33 . 1.420(3) no C32 C36 . 1.498(2) no C33 C34 . 1.406(3) no C33 C37 . 1.505(2) no C34 C38 . 1.502(3) no C35 H35A . .9600 no C35 H35B . .9600 no C35 H35C . .9600 no C36 H36A . .9600 no C36 H36B . .9600 no C36 H36C . .9600 no C37 H37A . .9600 no C37 H37B . .9600 no C37 H37C . .9600 no C38 H38A . .9600 no C38 H38B . .9600 no C38 H38C . .9600 no C40 C44 . 1.416(2) no C40 C41 . 1.421(3) no C40 H40 . .9300 no C41 C42 . 1.413(2) no C41 C45 . 1.506(2) no C42 C43 . 1.413(2) no C42 C46 . 1.500(3) no C43 C44 . 1.415(2) no C43 C47 . 1.504(2) no C44 C48 . 1.500(2) no C45 H45A . .9600 no C45 H45B . .9600 no C45 H45C . .9600 no C46 H46A . .9600 no C46 H46B . .9600 no C46 H46C . .9600 no C47 H47A . .9600 no C47 H47B . .9600 no C47 H47C . .9600 no C48 H48A . .9600 no C48 H48B . .9600 no C48 H48C . .9600 no loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe .3463 .8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti .2776 .4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 O1 Ti O2 60.85(4) yes C6 P C12 100.71(8) yes C6 P C18 100.52(8) yes C12 P C18 101.96(8) yes C11 O1 Ti 89.68(9) yes C11 O2 Ti 89.35(9) yes C2 C1 C5 107.87(15) no C2 C1 C11 125.91(15) no C5 C1 C11 126.17(15) no C3 C2 C1 108.06(16) no C3 C2 H2 126.0 no C1 C2 H2 126.0 no C2 C3 C4 108.24(16) no C2 C3 H3 125.9 no C4 C3 H3 125.9 no C3 C4 C5 108.30(16) no C3 C4 H4 125.8 no C5 C4 H4 125.8 no C4 C5 C1 107.52(16) no C4 C5 H5 126.2 no C1 C5 H5 126.2 no C10 C6 C7 106.90(14) no C10 C6 P 129.47(13) no C7 C6 P 123.63(13) no C8 C7 C6 108.23(15) no C8 C7 H7 125.9 no C6 C7 H7 125.9 no C7 C8 C9 108.29(15) no C7 C8 H8 125.9 no C9 C8 H8 125.9 no C10 C9 C8 107.97(15) no C10 C9 H9 126.0 no C8 C9 H9 126.0 no C9 C10 C6 108.61(15) no C9 C10 H10 125.7 no C6 C10 H10 125.7 no O2 C11 O1 119.18(14) yes O2 C11 C1 121.10(14) yes O1 C11 C1 119.59(14) yes C13 C12 C17 118.40(17) no C13 C12 P 117.55(14) no C17 C12 P 124.02(14) no C14 C13 C12 121.0(2) no C14 C13 H13 119.5 no C12 C13 H13 119.5 no C15 C14 C13 120.2(2) no C15 C14 H14 119.9 no C13 C14 H14 119.9 no C14 C15 C16 120.0(2) no C14 C15 H15 120.0 no C16 C15 H15 120.0 no C15 C16 C17 120.2(2) no C15 C16 H16 119.9 no C17 C16 H16 119.9 no C16 C17 C12 120.17(19) no C16 C17 H17 119.9 no C12 C17 H17 119.9 no C23 C18 C19 118.20(16) no C23 C18 P 123.72(13) no C19 C18 P 117.85(13) no C20 C19 C18 120.65(18) no C20 C19 H19 119.7 no C18 C19 H19 119.7 no C21 C20 C19 120.47(17) no C21 C20 H20 119.8 no C19 C20 H20 119.8 no C20 C21 C22 119.54(17) no C20 C21 H21 120.2 no C22 C21 H21 120.2 no C21 C22 C23 120.18(18) no C21 C22 H22 119.9 no C23 C22 H22 119.9 no C18 C23 C22 120.96(17) no C18 C23 H23 119.5 no C22 C23 H23 119.5 no C31 C30 C34 109.65(15) no C31 C30 H30 125.2 no C34 C30 H30 125.2 no C30 C31 C32 106.76(15) no C30 C31 C35 126.36(16) no C32 C31 C35 126.87(16) no C33 C32 C31 108.12(15) no C33 C32 C36 125.39(16) no C31 C32 C36 126.39(17) no C34 C33 C32 108.50(15) no C34 C33 C37 126.40(18) no C32 C33 C37 125.07(17) no C33 C34 C30 106.96(15) no C33 C34 C38 126.58(17) no C30 C34 C38 126.28(17) no C31 C35 H35A 109.5 no C31 C35 H35B 109.5 no H35A C35 H35B 109.5 no C31 C35 H35C 109.5 no H35A C35 H35C 109.5 no H35B C35 H35C 109.5 no C32 C36 H36A 109.5 no C32 C36 H36B 109.5 no H36A C36 H36B 109.5 no C32 C36 H36C 109.5 no H36A C36 H36C 109.5 no H36B C36 H36C 109.5 no C33 C37 H37A 109.5 no C33 C37 H37B 109.5 no H37A C37 H37B 109.5 no C33 C37 H37C 109.5 no H37A C37 H37C 109.5 no H37B C37 H37C 109.5 no C34 C38 H38A 109.5 no C34 C38 H38B 109.5 no H38A C38 H38B 109.5 no C34 C38 H38C 109.5 no H38A C38 H38C 109.5 no H38B C38 H38C 109.5 no C44 C40 C41 108.95(15) no C44 C40 H40 125.5 no C41 C40 H40 125.5 no Ti C40 H40 118.6 no C42 C41 C40 107.21(15) no C42 C41 C45 126.29(17) no C40 C41 C45 126.18(16) no C43 C42 C41 108.12(15) no C43 C42 C46 125.98(16) no C41 C42 C46 125.87(16) no C42 C43 C44 108.82(14) no C42 C43 C47 126.25(16) no C44 C43 C47 124.78(16) no C43 C44 C40 106.87(15) no C43 C44 C48 125.59(16) no C40 C44 C48 127.47(16) no C41 C45 H45A 109.5 no C41 C45 H45B 109.5 no H45A C45 H45B 109.5 no C41 C45 H45C 109.5 no H45A C45 H45C 109.5 no H45B C45 H45C 109.5 no C42 C46 H46A 109.5 no C42 C46 H46B 109.5 no H46A C46 H46B 109.5 no C42 C46 H46C 109.5 no H46A C46 H46C 109.5 no H46B C46 H46C 109.5 no C43 C47 H47A 109.5 no C43 C47 H47B 109.5 no H47A C47 H47B 109.5 no C43 C47 H47C 109.5 no H47A C47 H47C 109.5 no H47B C47 H47C 109.5 no C44 C48 H48A 109.5 no C44 C48 H48B 109.5 no H48A C48 H48B 109.5 no C44 C48 H48C 109.5 no H48A C48 H48C 109.5 no H48B C48 H48C 109.5 no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_publ_flag O1 Ti O2 C11 5.62(8) no C5 C1 C2 C3 .07(18) no C11 C1 C2 C3 177.63(15) no C1 C2 C3 C4 -.34(19) no C2 C3 C4 C5 .5(2) no C3 C4 C5 C1 -.43(19) no C2 C1 C5 C4 .22(18) no C11 C1 C5 C4 -177.33(15) no C18 P C6 C10 -89.32(16) no C12 P C6 C10 15.14(17) no C18 P C6 C7 90.99(14) no C12 P C6 C7 -164.56(14) no C10 C6 C7 C8 .02(18) no P C6 C7 C8 179.78(12) no C6 C7 C8 C9 -.27(19) no C7 C8 C9 C10 .42(19) no C8 C9 C10 C6 -.41(19) no C7 C6 C10 C9 .24(18) no P C6 C10 C9 -179.50(12) no Ti O2 C11 O1 -9.59(14) no Ti O1 C11 C1 -166.29(13) yes Ti O2 C11 C1 166.26(13) yes Ti O1 C11 O2 9.62(14) no C2 C1 C11 O2 165.14(15) no C2 C1 C11 O1 -19.0(2) yes C5 C1 C11 O2 -17.7(2) yes C5 C1 C11 O1 158.10(15) no C2 C1 C11 Ti -102.5(6) no C5 C1 C11 Ti 74.6(6) no O1 Ti C11 O2 -170.31(14) no O2 Ti C11 O1 170.31(14) no O1 Ti C11 C1 90.4(6) no O2 Ti C11 C1 -99.3(6) no C6 P C12 C13 103.49(14) no C18 P C12 C13 -153.22(13) no C6 P C12 C17 -74.77(15) no C18 P C12 C17 28.53(16) no C17 C12 C13 C14 1.8(3) no P C12 C13 C14 -176.57(15) no C12 C13 C14 C15 -1.3(3) no C13 C14 C15 C16 .0(3) no C14 C15 C16 C17 .9(3) no C15 C16 C17 C12 -.4(3) no C13 C12 C17 C16 -.9(3) no P C12 C17 C16 177.31(13) no C6 P C18 C23 -8.74(17) no C12 P C18 C23 -112.18(16) no C6 P C18 C19 176.97(14) no C12 P C18 C19 73.53(15) no C23 C18 C19 C20 .4(3) no P C18 C19 C20 174.99(15) no C18 C19 C20 C21 -.8(3) no C19 C20 C21 C22 .7(3) no C20 C21 C22 C23 -.3(3) no C19 C18 C23 C22 .1(3) no P C18 C23 C22 -174.19(14) no C21 C22 C23 C18 -.1(3) no C34 C30 C31 C35 178.71(16) no C30 C31 C32 C33 .26(18) no C35 C31 C32 C33 -178.54(16) no C30 C31 C32 C36 176.77(16) no C35 C31 C32 C36 -2.0(3) no C31 C32 C33 C34 -.33(18) no C36 C32 C33 C34 -176.89(16) no C31 C32 C33 C37 177.95(16) no C36 C32 C33 C37 1.4(3) no C32 C33 C34 C30 .27(18) no C37 C33 C34 C30 -177.99(16) no C32 C33 C34 C38 175.50(16) no C37 C33 C34 C38 -2.8(3) no C31 C30 C34 C33 -.10(19) no C31 C30 C34 C38 -175.36(16) no C44 C40 C41 C42 -1.55(18) no C44 C40 C41 C45 -175.25(16) no C40 C41 C42 C43 1.14(18) no C45 C41 C42 C43 174.84(16) no C40 C41 C42 C46 -177.17(16) no C45 C41 C42 C46 -3.5(3) no C41 C42 C43 C44 -.33(18) no C46 C42 C43 C44 177.98(16) no C41 C42 C43 C47 -176.09(15) no C46 C42 C43 C47 2.2(3) no C42 C43 C44 C40 -.62(18) no C47 C43 C44 C40 175.22(15) no C42 C43 C44 C48 -177.76(15) no C47 C43 C44 C48 -1.9(3) no C41 C40 C44 C43 1.34(18) no C41 C40 C44 C48 178.41(16) no _cod_database_fobs_code 2012498 _journal_paper_doi 10.1107/S0108270101019370