#------------------------------------------------------------------------------
#$Date: 2016-02-16 18:55:33 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176466 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/11/8101102.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_8101102
loop_
_publ_author_name
'Spannenberg, Anke'
'Burlakov, Vladimir V.'
'Rosenthal, Uwe'
_publ_section_title
;
Crystal structure of [2,2-bis(η⁵-pentamethylcyclopentadienyl)-
bis-(μ,η¹:η²-2-trimethylsilyl-ethinyl)titanium(IV) lithium]
[2,2-bis(η⁵-pentamethylcyclopentadienyl)-oxotitanium(III)---
tetrahydrofurane (1/0.5), C₅₀H₇₈LiOSi₂Ti₂ · 0.5C₄H₈O
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              616
_journal_page_last               618
_journal_volume                  216
_journal_year                    2001
_chemical_formula_structural     'C50 H78 LiO Si2 Ti2 . 0.5 C4 H8 O'
_chemical_formula_sum            'C52 H82 Li O1.5 Si2 Ti2'
_chemical_formula_weight         890.10
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 100.36(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.314(2)
_cell_length_b                   23.451(5)
_cell_length_c                   23.651(5)
_cell_measurement_temperature    200(2)
_cell_volume                     5627.3(20)
_diffrn_ambient_temperature      200(2)
_exptl_crystal_density_diffrn    1.051
_refine_ls_R_factor_obs          0.0640
_refine_ls_wR_factor_obs         0.1601
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C52 H82 Li O1.50 Si2 Ti2'
_cod_database_code               8101102
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
C1 C 1.0262(7) 0.3720(3) 0.6688(3) 0.038(2) Uani 1 d . .
C2 C 0.9281(6) 0.3600(3) 0.7017(3) 0.038(2) Uani 1 d . .
C3 C 0.9588(6) 0.3903(3) 0.7546(3) 0.035(2) Uani 1 d . .
C4 C 1.0758(6) 0.4209(3) 0.7542(3) 0.036(2) Uani 1 d . .
C5 C 1.1148(6) 0.4111(3) 0.7000(3) 0.034(2) Uani 1 d . .
C6 C 1.2136(7) 0.4465(3) 0.6756(3) 0.053(2) Uani 1 d . .
H6A H 1.2637(7) 0.4701(3) 0.7060(3) 0.080 Uiso 1 calc R .
H6B H 1.1672(7) 0.4710(3) 0.6450(3) 0.080 Uiso 1 calc R .
H6C H 1.2740(7) 0.4212(3) 0.6599(3) 0.080 Uiso 1 calc R .
C7 C 1.3409(7) 0.3068(4) 0.7174(4) 0.046(2) Uani 1 d . .
C8 C 1.3731(6) 0.3365(3) 0.7701(4) 0.041(2) Uani 1 d . .
C9 C 1.3373(7) 0.3021(4) 0.8134(3) 0.048(2) Uani 1 d . .
C10 C 1.2880(7) 0.2510(4) 0.7887(4) 0.052(2) Uani 1 d . .
C11 C 1.2850(7) 0.2540(4) 0.7284(4) 0.054(2) Uani 1 d . .
C44 C 1.3840(8) 0.3223(5) 0.6611(4) 0.085(3) Uani 1 d . .
H44A H 1.3483(8) 0.2944(5) 0.6315(4) 0.128 Uiso 1 calc R .
H44B H 1.4805(8) 0.3222(5) 0.6665(4) 0.128 Uiso 1 calc R .
H44C H 1.3510(8) 0.3604(5) 0.6489(4) 0.128 Uiso 1 calc R .
C47 C 1.4520(7) 0.3903(4) 0.7801(4) 0.073(3) Uani 1 d . .
H47A H 1.4594(7) 0.4019(4) 0.8204(4) 0.109 Uiso 1 calc R .
H47B H 1.4079(7) 0.4205(4) 0.7551(4) 0.109 Uiso 1 calc R .
H47C H 1.5402(7) 0.3838(4) 0.7714(4) 0.109 Uiso 1 calc R .
C46 C 1.3631(8) 0.3169(5) 0.8765(4) 0.095(4) Uani 1 d . .
H46A H 1.3982(8) 0.3557(5) 0.8818(4) 0.143 Uiso 1 calc R .
H46B H 1.4273(8) 0.2900(5) 0.8974(4) 0.143 Uiso 1 calc R .
H46C H 1.2806(8) 0.3145(5) 0.8915(4) 0.143 Uiso 1 calc R .
C49 C 1.2504(8) 0.2002(4) 0.8206(5) 0.108(4) Uani 1 d . .
H49A H 1.2180(8) 0.1699(4) 0.7932(5) 0.161 Uiso 1 calc R .
H49B H 1.1809(8) 0.2110(4) 0.8418(5) 0.161 Uiso 1 calc R .
H49C H 1.3276(8) 0.1866(4) 0.8475(5) 0.161 Uiso 1 calc R .
C12 C 1.2484(9) 0.2072(5) 0.6854(5) 0.124(5) Uani 1 d . .
H12A H 1.2555(9) 0.2211(5) 0.6470(5) 0.187 Uiso 1 calc R .
H12B H 1.1576(9) 0.1951(5) 0.6857(5) 0.187 Uiso 1 calc R .
H12C H 1.3082(9) 0.1748(5) 0.6954(5) 0.187 Uiso 1 calc R .
C13 C 0.6298(6) 0.1835(3) 0.9148(3) 0.039(2) Uani 1 d . .
C14 C 0.6583(6) 0.2108(3) 0.8645(4) 0.041(2) Uani 1 d . .
C15 C 0.6177(7) 0.1759(4) 0.8182(3) 0.045(2) Uani 1 d . .
C16 C 0.5633(7) 0.1261(4) 0.8366(3) 0.044(2) Uani 1 d . .
C17 C 0.5654(6) 0.1317(3) 0.8970(3) 0.040(2) Uani 1 d . .
C18 C 0.4882(7) 0.0972(4) 0.9325(4) 0.069(3) Uani 1 d . .
H18A H 0.4529(7) 0.0632(4) 0.9109(4) 0.103 Uiso 1 calc R .
H18B H 0.4153(7) 0.1202(4) 0.9416(4) 0.103 Uiso 1 calc R .
H18C H 0.5458(7) 0.0856(4) 0.9682(4) 0.103 Uiso 1 calc R .
C19 C 0.9802(7) 0.0603(3) 0.9046(4) 0.042(2) Uani 1 d . .
C20 C 0.8742(8) 0.0275(3) 0.8768(3) 0.043(2) Uani 1 d . .
C21 C 0.7801(6) 0.0233(3) 0.9130(3) 0.040(2) Uani 1 d . .
C22 C 0.8276(7) 0.0544(3) 0.9641(3) 0.040(2) Uani 1 d . .
C23 C 0.9502(7) 0.0764(3) 0.9585(4) 0.049(2) Uani 1 d . .
C24 C 1.0432(9) 0.1048(4) 1.0080(4) 0.087(3) Uani 1 d . .
H24A H 1.1236(9) 0.1169(4) 0.9947(4) 0.130 Uiso 1 calc R .
H24B H 1.0660(9) 0.0775(4) 1.0396(4) 0.130 Uiso 1 calc R .
H24C H 0.9998(9) 0.1380(4) 1.0213(4) 0.130 Uiso 1 calc R .
C25 C 0.9272(6) 0.1893(3) 0.9130(3) 0.030(2) Uani 1 d . .
C26 C 1.0039(7) 0.2270(3) 0.9348(3) 0.038(2) Uani 1 d . .
C27 C 0.8584(6) 0.1262(3) 0.8027(3) 0.032(2) Uani 1 d . .
C28 C 0.8916(7) 0.1244(3) 0.7547(3) 0.039(2) Uani 1 d . .
C29 C 1.2723(7) 0.2465(3) 1.0047(3) 0.053(2) Uani 1 d . .
H29A H 1.3261(7) 0.2718(3) 1.0324(3) 0.079 Uiso 1 calc R .
H29B H 1.3106(7) 0.2441(3) 0.9697(3) 0.079 Uiso 1 calc R .
H29C H 1.2698(7) 0.2084(3) 1.0215(3) 0.079 Uiso 1 calc R .
C30 C 1.0969(8) 0.3497(3) 0.9587(4) 0.068(3) Uani 1 d . .
H30A H 1.1502(8) 0.3745(3) 0.9872(4) 0.102 Uiso 1 calc R .
H30B H 1.0056(8) 0.3633(3) 0.9513(4) 0.102 Uiso 1 calc R .
H30C H 1.1321(8) 0.3506(3) 0.9229(4) 0.102 Uiso 1 calc R .
C31 C 1.0299(8) 0.2753(4) 1.0534(4) 0.080(3) Uani 1 d . .
H31A H 1.0811(8) 0.3008(4) 1.0818(4) 0.120 Uiso 1 calc R .
H31B H 1.0322(8) 0.2366(4) 1.0690(4) 0.120 Uiso 1 calc R .
H31C H 0.9384(8) 0.2886(4) 1.0444(4) 0.120 Uiso 1 calc R .
C32 C 0.8971(9) 0.1648(4) 0.6341(4) 0.085(3) Uani 1 d . .
H32A H 0.9025(9) 0.1519(4) 0.5952(4) 0.127 Uiso 1 calc R .
H32B H 0.9719(9) 0.1899(4) 0.6484(4) 0.127 Uiso 1 calc R .
H32C H 0.8146(9) 0.1857(4) 0.6334(4) 0.127 Uiso 1 calc R .
C33 C 1.0527(10) 0.0598(4) 0.6816(4) 0.091(3) Uani 1 d . .
H33A H 1.0565(10) 0.0483(4) 0.6421(4) 0.137 Uiso 1 calc R .
H33B H 1.0510(10) 0.0258(4) 0.7055(4) 0.137 Uiso 1 calc R .
H33C H 1.1304(10) 0.0829(4) 0.6969(4) 0.137 Uiso 1 calc R .
C34 C 0.7572(11) 0.0574(5) 0.6548(5) 0.124(4) Uani 1 d . .
H34A H 0.7609(11) 0.0452(5) 0.6156(5) 0.186 Uiso 1 calc R .
H34B H 0.6763(11) 0.0793(5) 0.6549(5) 0.186 Uiso 1 calc R .
H34C H 0.7577(11) 0.0239(5) 0.6796(5) 0.186 Uiso 1 calc R .
C35 C 0.6481(7) 0.2090(4) 0.9741(3) 0.057(2) Uani 1 d . .
H35A H 0.6962(7) 0.2450(4) 0.9747(3) 0.085 Uiso 1 calc R .
H35B H 0.6982(7) 0.1825(4) 1.0018(3) 0.085 Uiso 1 calc R .
H35C H 0.5617(7) 0.2160(4) 0.9845(3) 0.085 Uiso 1 calc R .
C36 C 1.0275(8) 0.3525(4) 0.6081(3) 0.059(2) Uani 1 d . .
H36A H 0.9553(8) 0.3254(4) 0.5962(3) 0.088 Uiso 1 calc R .
H36B H 1.1118(8) 0.3339(4) 0.6064(3) 0.088 Uiso 1 calc R .
H36C H 1.0162(8) 0.3855(4) 0.5823(3) 0.088 Uiso 1 calc R .
C37 C 0.6146(8) 0.1936(5) 0.7563(4) 0.088(3) Uani 1 d . .
H37A H 0.5822(8) 0.1618(5) 0.7307(4) 0.132 Uiso 1 calc R .
H37B H 0.7037(8) 0.2039(5) 0.7510(4) 0.132 Uiso 1 calc R .
H37C H 0.5559(8) 0.2264(5) 0.7471(4) 0.132 Uiso 1 calc R .
C38 C 1.1086(7) 0.0725(4) 0.8846(5) 0.087(3) Uani 1 d . .
H38A H 1.1643(7) 0.0966(4) 0.9129(5) 0.130 Uiso 1 calc R .
H38B H 1.0905(7) 0.0921(4) 0.8474(5) 0.130 Uiso 1 calc R .
H38C H 1.1544(7) 0.0365(4) 0.8804(5) 0.130 Uiso 1 calc R .
C39 C 0.8732(10) -0.0062(4) 0.8223(4) 0.079(3) Uani 1 d . .
H39A H 0.7881(10) -0.0255(4) 0.8114(4) 0.119 Uiso 1 calc R .
H39B H 0.9439(10) -0.0347(4) 0.8287(4) 0.119 Uiso 1 calc R .
H39C H 0.8871(10) 0.0197(4) 0.7914(4) 0.119 Uiso 1 calc R .
C40 C 0.4956(8) 0.0795(4) 0.7982(4) 0.078(3) Uani 1 d . .
H40A H 0.4662(8) 0.0495(4) 0.8218(4) 0.116 Uiso 1 calc R .
H40B H 0.5574(8) 0.0634(4) 0.7754(4) 0.116 Uiso 1 calc R .
H40C H 0.4193(8) 0.0954(4) 0.7723(4) 0.116 Uiso 1 calc R .
C41 C 1.1340(7) 0.4625(3) 0.8012(3) 0.053(2) Uani 1 d . .
H41A H 1.2151(7) 0.4790(3) 0.7921(3) 0.079 Uiso 1 calc R .
H41B H 1.1540(7) 0.4424(3) 0.8381(3) 0.079 Uiso 1 calc R .
H41C H 1.0703(7) 0.4930(3) 0.8037(3) 0.079 Uiso 1 calc R .
C42 C 0.7065(7) 0.2709(4) 0.8608(4) 0.076(3) Uani 1 d . .
H42A H 0.7296(7) 0.2870(4) 0.8996(4) 0.114 Uiso 1 calc R .
H42B H 0.6368(7) 0.2940(4) 0.8381(4) 0.114 Uiso 1 calc R .
H42C H 0.7844(7) 0.2710(4) 0.8425(4) 0.114 Uiso 1 calc R .
C43 C 0.8772(7) 0.3926(3) 0.8016(3) 0.055(2) Uani 1 d . .
H43A H 0.8008(7) 0.3673(3) 0.7917(3) 0.082 Uiso 1 calc R .
H43B H 0.8468(7) 0.4317(3) 0.8055(3) 0.082 Uiso 1 calc R .
H43C H 0.9309(7) 0.3802(3) 0.8379(3) 0.082 Uiso 1 calc R .
C45 C 0.8064(7) 0.3240(3) 0.6816(4) 0.057(2) Uani 1 d . .
H45A H 0.8099(7) 0.3082(3) 0.6435(4) 0.085 Uiso 1 calc R .
H45B H 0.7274(7) 0.3477(3) 0.6794(4) 0.085 Uiso 1 calc R .
H45C H 0.8032(7) 0.2928(3) 0.7088(4) 0.085 Uiso 1 calc R .
C48 C 0.6666(7) -0.0189(4) 0.9036(4) 0.075(3) Uani 1 d . .
H48A H 0.6139(7) -0.0142(4) 0.9338(4) 0.112 Uiso 1 calc R .
H48B H 0.7015(7) -0.0578(4) 0.9048(4) 0.112 Uiso 1 calc R .
H48C H 0.6111(7) -0.0119(4) 0.8660(4) 0.112 Uiso 1 calc R .
C50 C 0.7727(9) 0.0554(4) 1.0184(4) 0.080(3) Uani 1 d . .
H50A H 0.6851(9) 0.0377(4) 1.0116(4) 0.120 Uiso 1 calc R .
H50B H 0.7657(9) 0.0949(4) 1.0309(4) 0.120 Uiso 1 calc R .
H50C H 0.8312(9) 0.0341(4) 1.0483(4) 0.120 Uiso 1 calc R .
Li Li 0.9872(11) 0.2032(5) 0.8284(5) 0.044(3) Uani 1 d . .
O1 O 1.0224(4) 0.2710(2) 0.7870(2) 0.0543(15) Uani 1 d . .
O2 O 0.7159(4) 0.3849(2) 1.0491(2) 0.153(7) Uiso 0.50 d PR .
C52 C 0.6736(4) 0.3915(2) 0.9889(2) 0.106(7) Uiso 0.50 d PR .
H52A H 0.6949(4) 0.3568(2) 0.9686(2) 0.127 Uiso 0.50 calc PR .
H52B H 0.5771(4) 0.3975(2) 0.9801(2) 0.127 Uiso 0.50 calc PR .
C53 C 0.7399(4) 0.4394(2) 0.9710(2) 0.199(14) Uiso 0.50 d PR .
H53A H 0.6751(4) 0.4684(2) 0.9535(2) 0.238 Uiso 0.50 calc PR .
H53B H 0.7930(4) 0.4277(2) 0.9420(2) 0.238 Uiso 0.50 calc PR .
C54 C 0.8231(4) 0.4625(2) 1.0200(2) 0.202(15) Uiso 0.50 d PR .
H54A H 0.9160(4) 0.4618(2) 1.0146(2) 0.243 Uiso 0.50 calc PR .
H54B H 0.7982(4) 0.5025(2) 1.0261(2) 0.243 Uiso 0.50 calc PR .
C55 C 0.8082(4) 0.4288(2) 1.0683(2) 0.103(7) Uiso 0.50 d PR .
H55A H 0.7762(4) 0.4526(2) 1.0975(2) 0.123 Uiso 0.50 calc PR .
H55B H 0.8940(4) 0.4119(2) 1.0860(2) 0.123 Uiso 0.50 calc PR .
Si1 Si 1.1023(2) 0.27525(9) 0.98651(9) 0.0421(6) Uani 1 d . .
Si2 Si 0.9016(2) 0.10243(11) 0.68214(10) 0.0572(7) Uani 1 d . .
Ti1 Ti 1.13466(11) 0.32275(5) 0.75185(5) 0.0335(4) Uani 1 d . .
Ti2 Ti 0.79143(11) 0.12281(5) 0.88326(5) 0.0291(4) Uani 1 d . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C5 1.408(9) . ?
C1 C2 1.412(9) . ?
C1 C36 1.507(10) . ?
C1 Ti1 2.378(7) . ?
C2 C3 1.424(9) . ?
C2 C45 1.517(10) . ?
C2 Ti1 2.409(7) . ?
C3 C4 1.405(9) . ?
C3 C43 1.510(9) . ?
C3 Ti1 2.418(6) . ?
C4 C5 1.429(9) . ?
C4 C41 1.519(10) . ?
C4 Ti1 2.383(7) . ?
C5 C6 1.507(9) . ?
C5 Ti1 2.397(7) . ?
C7 C8 1.414(10) . ?
C7 C11 1.409(11) . ?
C7 C44 1.522(10) . ?
C7 Ti1 2.440(7) . ?
C8 C9 1.405(10) . ?
C8 C47 1.498(10) . ?
C8 Ti1 2.441(7) . ?
C9 C10 1.390(11) . ?
C9 C46 1.508(11) . ?
C9 Ti1 2.373(7) . ?
C10 C11 1.423(11) . ?
C10 C49 1.498(11) . ?
C10 Ti1 2.365(7) . ?
C11 C12 1.497(12) . ?
C11 Ti1 2.371(7) . ?
C13 C17 1.412(10) . ?
C13 C14 1.428(10) . ?
C13 C35 1.505(10) . ?
C13 Ti2 2.410(7) . ?
C14 C15 1.371(10) . ?
C14 C42 1.502(10) . ?
C14 Ti2 2.475(7) . ?
C15 C16 1.399(11) . ?
C15 C37 1.517(10) . ?
C15 Ti2 2.477(7) . ?
C16 C17 1.430(10) . ?
C16 C40 1.508(11) . ?
C16 Ti2 2.414(7) . ?
C17 C18 1.495(10) . ?
C17 Ti2 2.420(6) . ?
C19 C20 1.400(10) . ?
C19 C23 1.415(10) . ?
C19 C38 1.513(10) . ?
C19 Ti2 2.417(7) . ?
C20 C21 1.408(10) . ?
C20 C39 1.511(10) . ?
C20 Ti2 2.408(7) . ?
C21 C22 1.420(10) . ?
C21 C48 1.519(10) . ?
C21 Ti2 2.445(7) . ?
C22 C23 1.394(10) . ?
C22 C50 1.494(10) . ?
C22 Ti2 2.473(7) . ?
C23 C24 1.527(10) . ?
C23 Ti2 2.446(7) . ?
C25 C26 1.236(9) . ?
C25 Ti2 2.129(8) . ?
C25 Li 2.224(14) . ?
C26 Si1 1.832(8) . ?
C26 Li 2.554(14) . ?
C27 C28 1.242(9) . ?
C27 Ti2 2.143(8) . ?
C27 Li 2.259(14) . ?
C28 Si2 1.813(8) . ?
C28 Li 2.608(15) . ?
C29 Si1 1.855(7) . ?
C30 Si1 1.864(8) . ?
C31 Si1 1.866(8) . ?
C32 Si2 1.847(8) . ?
C33 Si2 1.853(9) . ?
C34 Si2 1.844(10) . ?
Li O1 1.936(12) . ?
Li Ti2 3.203(12) . ?
O1 Ti1 1.962(4) . ?
O2 C52 1.42 . ?
O2 C55 1.42 . ?
C52 C53 1.42 . ?
C53 C54 1.42 . ?
C54 C55 1.42 . ?
