#------------------------------------------------------------------------------ #$Date: 2016-02-21 00:03:34 +0000 (Sun, 21 Feb 2016) $ #$Revision: 176798 $ #$URL: svn://www.crystallography.net/cod/cif/2/23/88/2238875.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_2238875 loop_ _publ_author_name 'Nielson, Alastair J.' 'Shen, Chaohong' 'Waters, Joyce M.' _publ_section_title ; Bis(\m-2-hydroxymethyl-2-methylpropane-1,3-diolato)bis[dichloridotitanium(IV)] diethyl ether disolvate ; _journal_coeditor_code HG5360 _journal_issue 12 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m676 _journal_page_last m677 _journal_paper_doi 10.1107/S1600536813031504 _journal_volume 69 _journal_year 2013 _chemical_formula_iupac '[Ti2 Cl4 (C5 H10 O3)2], 2C4 H10 O' _chemical_formula_moiety 'C10 H20 O6 Cl4 Ti2, 2(C4 H10 O)' _chemical_formula_sum 'C18 H40 Cl4 O8 Ti2' _chemical_formula_weight 622.10 _chemical_name_systematic ;Bis(\m-2-hydroxymethyl-2-methylpropane-1,3-diolato)bis[dichloridotitanium(IV)] diethyl ether disolvate ; _space_group_IT_number 2 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 71.3510(10) _cell_angle_beta 82.0230(10) _cell_angle_gamma 66.7570(10) _cell_formula_units_Z 1 _cell_length_a 7.9617(3) _cell_length_b 9.6379(4) _cell_length_c 10.5783(5) _cell_measurement_reflns_used 5595 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 25 _cell_measurement_theta_min 2 _cell_volume 706.60(5) _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_collection 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 2012)' _computing_publication_material 'SHELXL97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _diffrn_ambient_temperature 150(2) _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method 'Area detector \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0151 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 6510 _diffrn_reflns_theta_full 25.71 _diffrn_reflns_theta_max 25.71 _diffrn_reflns_theta_min 2.03 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 0.980 _exptl_absorpt_correction_T_max 0.8922 _exptl_absorpt_correction_T_min 0.7657 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Blessing, 1995)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.462 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 324 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.10 _refine_diff_density_max 0.312 _refine_diff_density_min -0.266 _refine_ls_extinction_coef 0 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 152 _refine_ls_number_reflns 2661 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0249 _refine_ls_R_factor_gt 0.0215 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0325P)^2^+0.2355P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.0606 _reflns_number_gt 2417 _reflns_number_total 2661 _reflns_threshold_expression I>2sigma(I) _cod_data_source_file hg5360.cif _cod_data_source_block I _cod_database_code 2238875 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_type_symbol _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_symmetry_multiplicity Ti Ti 0.58094(3) 0.61520(3) 0.39188(2) 0.01725(9) Uani d . 1 1 Cl Cl1 0.74357(5) 0.59557(5) 0.19464(4) 0.02805(11) Uani d . 1 1 Cl Cl2 0.47954(5) 0.88725(4) 0.35265(4) 0.02495(10) Uani d . 1 1 O O1 0.43149(13) 0.59722(11) 0.56614(9) 0.0177(2) Uani d . 1 1 O O2 0.76654(13) 0.57443(12) 0.48899(10) 0.0217(2) Uani d . 1 1 O O3 0.66826(14) 0.32177(13) 0.70683(10) 0.0197(2) Uani d . 1 1 C C1 0.4634(2) 0.65978(17) 0.66438(14) 0.0209(3) Uani d . 1 1 H H1A 0.3764 0.6490 0.7400 0.025 Uiso calc R 1 1 H H1B 0.4384 0.7737 0.6237 0.025 Uiso calc R 1 1 C C2 0.6586(2) 0.57709(17) 0.71785(15) 0.0211(3) Uani d . 1 1 C C3 0.7972(2) 0.60351(19) 0.60594(15) 0.0248(3) Uani d . 1 1 H H3A 0.7897 0.7137 0.5832 0.030 Uiso calc R 1 1 H H3B 0.9221 0.5328 0.6382 0.030 Uiso calc R 1 1 H H3 0.721(3) 0.236(3) 0.737(2) 0.038(6) Uiso d . 1 1 C C4 0.6997(2) 0.40296(17) 0.78961(15) 0.0227(3) Uani d . 1 1 H H4A 0.8288 0.3514 0.8178 0.027 Uiso calc R 1 1 H H4B 0.6216 0.3934 0.8709 0.027 Uiso calc R 1 1 C C5 0.6733(2) 0.65305(19) 0.82181(16) 0.0296(4) Uani d . 1 1 H H5A 0.5924 0.6323 0.8981 0.044 Uiso calc R 1 1 H H5B 0.6371 0.7672 0.7813 0.044 Uiso calc R 1 1 H H5C 0.7997 0.6079 0.8522 0.044 Uiso calc R 1 1 O O11 0.89033(14) 0.03405(12) 0.82316(10) 0.0220(2) Uani d . 1 1 C C11 0.7018(2) 0.0355(2) 1.01998(16) 0.0309(4) Uani d . 1 1 H H11A 0.7672 0.0891 1.0464 0.046 Uiso calc R 1 1 H H11B 0.6635 -0.0316 1.0999 0.046 Uiso calc R 1 1 H H11C 0.5939 0.1143 0.9687 0.046 Uiso calc R 1 1 C C12 0.8258(2) -0.06469(18) 0.93561(16) 0.0276(3) Uani d . 1 1 H H12A 0.9306 -0.1496 0.9889 0.033 Uiso calc R 1 1 H H12B 0.7584 -0.1142 0.9041 0.033 Uiso calc R 1 1 C C13 1.0030(2) -0.0498(2) 0.73231(17) 0.0305(4) Uani d . 1 1 H H13A 0.9318 -0.0910 0.6945 0.037 Uiso calc R 1 1 H H13B 1.1090 -0.1401 0.7797 0.037 Uiso calc R 1 1 C C14 1.0679(2) 0.0633(2) 0.62220(18) 0.0375(4) Uani d . 1 1 H H14A 0.9624 0.1497 0.5732 0.056 Uiso calc R 1 1 H H14B 1.1492 0.0074 0.5610 0.056 Uiso calc R 1 1 H H14C 1.1343 0.1064 0.6609 0.056 Uiso calc R 1 1 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 Ti 0.01564(14) 0.01876(14) 0.01493(14) -0.00583(10) 0.00015(10) -0.00266(10) Cl1 0.0258(2) 0.0379(2) 0.01864(19) -0.01292(16) 0.00543(15) -0.00699(16) Cl2 0.0292(2) 0.01963(18) 0.0251(2) -0.01055(15) -0.00415(15) -0.00208(14) O1 0.0167(5) 0.0178(5) 0.0160(5) -0.0040(4) 0.0002(4) -0.0047(4) O2 0.0178(5) 0.0266(5) 0.0192(5) -0.0073(4) -0.0004(4) -0.0058(4) O3 0.0222(5) 0.0149(5) 0.0202(5) -0.0041(4) -0.0047(4) -0.0046(4) C1 0.0239(7) 0.0196(7) 0.0181(7) -0.0051(6) 0.0006(6) -0.0084(6) C2 0.0241(7) 0.0200(7) 0.0196(7) -0.0070(6) -0.0026(6) -0.0070(6) C3 0.0248(8) 0.0308(8) 0.0221(8) -0.0129(6) -0.0025(6) -0.0078(6) C4 0.0273(8) 0.0217(7) 0.0188(7) -0.0074(6) -0.0051(6) -0.0057(6) C5 0.0405(9) 0.0274(8) 0.0245(8) -0.0122(7) -0.0050(7) -0.0108(7) O11 0.0222(5) 0.0197(5) 0.0201(5) -0.0051(4) 0.0000(4) -0.0042(4) C11 0.0341(9) 0.0376(9) 0.0224(8) -0.0189(8) 0.0021(7) -0.0046(7) C12 0.0321(9) 0.0237(8) 0.0244(8) -0.0124(7) -0.0032(7) 0.0002(6) C13 0.0270(8) 0.0294(8) 0.0296(9) -0.0014(7) -0.0008(7) -0.0130(7) C14 0.0289(9) 0.0492(11) 0.0312(9) -0.0110(8) 0.0069(7) -0.0151(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 '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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle O2 Ti O1 . 2_666 101.78(5) O2 Ti O1 . . 86.71(4) O1 Ti O1 2_666 . 76.83(4) O2 Ti O3 . 2_666 172.39(5) O1 Ti O3 2_666 2_666 80.17(4) O1 Ti O3 . 2_666 86.59(4) O2 Ti Cl1 . . 97.18(4) O1 Ti Cl1 2_666 . 93.21(3) O1 Ti Cl1 . . 169.89(3) O3 Ti Cl1 2_666 . 90.02(3) O2 Ti Cl2 . . 93.95(4) O1 Ti Cl2 2_666 . 158.75(3) O1 Ti Cl2 . . 90.05(3) O3 Ti Cl2 2_666 . 82.46(3) Cl1 Ti Cl2 . . 98.956(16) O2 Ti Ti . 2_666 95.24(4) O1 Ti Ti 2_666 2_666 39.05(3) O1 Ti Ti . 2_666 37.78(3) O3 Ti Ti 2_666 2_666 81.61(3) Cl1 Ti Ti . 2_666 132.238(18) Cl2 Ti Ti . 2_666 125.940(16) C1 O1 Ti . 2_666 124.13(8) C1 O1 Ti . . 118.13(8) Ti O1 Ti 2_666 . 103.17(4) C3 O2 Ti . . 138.33(9) C4 O3 Ti . 2_666 126.66(9) C4 O3 H3 . . 106.5(16) Ti O3 H3 2_666 . 117.1(16) O1 C1 C2 . . 113.32(11) O1 C1 H1A . . 108.9 C2 C1 H1A . . 108.9 O1 C1 H1B . . 108.9 C2 C1 H1B . . 108.9 H1A C1 H1B . . 107.7 C4 C2 C1 . . 110.95(12) C4 C2 C3 . . 112.76(13) C1 C2 C3 . . 110.72(12) C4 C2 C5 . . 107.06(12) C1 C2 C5 . . 108.02(12) C3 C2 C5 . . 107.07(13) O2 C3 C2 . . 112.41(12) O2 C3 H3A . . 109.1 C2 C3 H3A . . 109.1 O2 C3 H3B . . 109.1 C2 C3 H3B . . 109.1 H3A C3 H3B . . 107.9 O3 C4 C2 . . 112.55(12) O3 C4 H4A . . 109.1 C2 C4 H4A . . 109.1 O3 C4 H4B . . 109.1 C2 C4 H4B . . 109.1 H4A C4 H4B . . 107.8 C2 C5 H5A . . 109.5 C2 C5 H5B . . 109.5 H5A C5 H5B . . 109.5 C2 C5 H5C . . 109.5 H5A C5 H5C . . 109.5 H5B C5 H5C . . 109.5 C13 O11 C12 . . 112.91(12) C12 C11 H11A . . 109.5 C12 C11 H11B . . 109.5 H11A C11 H11B . . 109.5 C12 C11 H11C . . 109.5 H11A C11 H11C . . 109.5 H11B C11 H11C . . 109.5 O11 C12 C11 . . 108.69(13) O11 C12 H12A . . 110.0 C11 C12 H12A . . 110.0 O11 C12 H12B . . 110.0 C11 C12 H12B . . 110.0 H12A C12 H12B . . 108.3 O11 C13 C14 . . 108.13(14) O11 C13 H13A . . 110.1 C14 C13 H13A . . 110.1 O11 C13 H13B . . 110.1 C14 C13 H13B . . 110.1 H13A C13 H13B . . 108.4 C13 C14 H14A . . 109.5 C13 C14 H14B . . 109.5 H14A C14 H14B . . 109.5 C13 C14 H14C . . 109.5 H14A C14 H14C . . 109.5 H14B C14 H14C . . 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance Ti O2 . 1.7601(10) Ti O1 2_666 1.9911(10) Ti O1 . 2.0478(10) Ti O3 2_666 2.1481(11) Ti Cl1 . 2.3184(4) Ti Cl2 . 2.3292(4) Ti Ti 2_666 3.1649(5) O1 C1 . 1.4501(17) O1 Ti 2_666 1.9911(10) O2 C3 . 1.4243(18) O3 C4 . 1.4473(18) O3 Ti 2_666 2.1481(11) O3 H3 . 0.74(2) C1 C2 . 1.533(2) C1 H1A . 0.9900 C1 H1B . 0.9900 C2 C4 . 1.523(2) C2 C3 . 1.533(2) C2 C5 . 1.542(2) C3 H3A . 0.9900 C3 H3B . 0.9900 C4 H4A . 0.9900 C4 H4B . 0.9900 C5 H5A . 0.9800 C5 H5B . 0.9800 C5 H5C . 0.9800 O11 C13 . 1.4374(19) O11 C12 . 1.4413(18) C11 C12 . 1.502(2) C11 H11A . 0.9800 C11 H11B . 0.9800 C11 H11C . 0.9800 C12 H12A . 0.9900 C12 H12B . 0.9900 C13 C14 . 1.509(3) C13 H13A . 0.9900 C13 H13B . 0.9900 C14 H14A . 0.9800 C14 H14B . 0.9800 C14 H14C . 0.9800 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA O3 H3 O11 0.74(2) 1.89(2) 2.6233(14) 168(2)