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#$Date: 2017-03-03 01:57:21 +0200 (Fri, 03 Mar 2017) $
#$Revision: 192790 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/53/4345304.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_4345304
loop_
_publ_author_name
'Petrus, Rafał'
'Utko, Józef'
'Lis, Tadeusz'
'Sobota, Piotr'
_publ_section_title
;
 Impact of Group 13 Metals on Cp2TiCl2 Reduction and Structural
 Characterization of Resulting Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_paper_doi               10.1021/acs.inorgchem.6b02824
_journal_year                    2017
_chemical_formula_moiety         'C16 H24 Cl2 O4 Ti2'
_chemical_formula_sum            'C16 H24 Cl2 O4 Ti2'
_chemical_formula_weight         446.99
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 101.98(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.6249(19)
_cell_length_b                   7.1156(18)
_cell_length_c                   15.685(5)
_cell_measurement_reflns_used    1624
_cell_measurement_temperature    80(2)
_cell_measurement_theta_max      30.6799
_cell_measurement_theta_min      2.8569
_cell_volume                     941.6(5)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2011)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2011)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2011)'
_computing_molecular_graphics    'DIAMOND  (Brandenburg, 2007)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      80(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3974
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         30.748
_diffrn_reflns_theta_min         2.987
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_T_max  0.946
_exptl_absorpt_correction_T_min  0.834
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_description       plate
_exptl_crystal_F_000             460
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.261
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     110
_refine_ls_number_reflns         2476
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0662
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0718P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1249
_refine_ls_wR_factor_ref         0.1342
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2074
_reflns_number_total             2476
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02824_si_001.cif
_cod_data_source_block           6A
_cod_database_code               4345304
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.803
_shelx_estimated_absorpt_t_max   0.977
loop_
_space_group_symop_operation_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_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
Ti1 Ti 0.43505(5) 0.53156(6) 0.58867(3) 0.01640(16) Uani 1 1 d . .
Cl1 Cl 0.27965(8) 0.25833(10) 0.60446(5) 0.0283(2) Uani 1 1 d . .
O1A O 0.4243(2) 0.6349(2) 0.47005(11) 0.0170(4) Uani 1 1 d . .
C1A C 0.3363(3) 0.8023(4) 0.44619(18) 0.0212(5) Uani 1 1 d . .
H1A1 H 0.3214 0.8234 0.3826 0.025 Uiso 1 1 calc R U
H1A2 H 0.3939 0.9114 0.4767 0.025 Uiso 1 1 calc R U
C2A C 0.1773(3) 0.7811(4) 0.4713(2) 0.0261(6) Uani 1 1 d . .
H2A1 H 0.1317 0.9060 0.4793 0.031 Uiso 1 1 calc R U
H2A2 H 0.1025 0.7124 0.4254 0.031 Uiso 1 1 calc R U
O2A O 0.2053(2) 0.6768(3) 0.55211(13) 0.0235(4) Uani 1 1 d . .
C3A C 0.0742(4) 0.6819(5) 0.5948(2) 0.0386(8) Uani 1 1 d . .
H3A1 H 0.0651 0.8080 0.6184 0.058 Uiso 1 1 calc R U
H3A2 H 0.0911 0.5901 0.6424 0.058 Uiso 1 1 calc R U
H3A3 H -0.0235 0.6511 0.5529 0.058 Uiso 1 1 calc R U
C11 C 0.5656(4) 0.5208(5) 0.73864(19) 0.0311(7) Uani 1 1 d . .
H11 H 0.5610 0.4115 0.7728 0.037 Uiso 1 1 calc R U
C21 C 0.4554(4) 0.6716(5) 0.72601(19) 0.0354(8) Uani 1 1 d . .
H21 H 0.3637 0.6813 0.7504 0.042 Uiso 1 1 calc R U
C31 C 0.5058(3) 0.8041(5) 0.6710(2) 0.0315(7) Uani 1 1 d . .
H31 H 0.4546 0.9196 0.6524 0.038 Uiso 1 1 calc R U
C41 C 0.6442(3) 0.7366(4) 0.6485(2) 0.0276(6) Uani 1 1 d . .
H41 H 0.7023 0.7967 0.6109 0.033 Uiso 1 1 calc R U
C51 C 0.6821(3) 0.5630(4) 0.69151(17) 0.0247(6) Uani 1 1 d . .
H51 H 0.7718 0.4874 0.6889 0.030 Uiso 1 1 calc R U
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1A Ti1 O1A 73.10(8) . 3_666
O1A Ti1 O2A 73.61(8) . .
O1A Ti1 O2A 137.72(8) 3_666 .
O1A Ti1 C31 99.59(10) . .
O1A Ti1 C31 128.13(9) 3_666 .
O2A Ti1 C31 82.66(10) . .
O1A Ti1 C21 133.09(11) . .
O1A Ti1 C21 136.12(10) 3_666 .
O2A Ti1 C21 86.07(10) . .
C31 Ti1 C21 34.91(12) . .
O1A Ti1 C41 91.51(10) . .
O1A Ti1 C41 93.51(9) 3_666 .
O2A Ti1 C41 112.70(10) . .
C31 Ti1 C41 34.65(11) . .
C21 Ti1 C41 57.79(12) . .
O1A Ti1 C11 148.82(10) . .
O1A Ti1 C11 102.85(10) 3_666 .
O2A Ti1 C11 119.07(10) . .
C31 Ti1 C11 57.81(11) . .
C21 Ti1 C11 34.88(11) . .
C41 Ti1 C11 57.52(11) . .
O1A Ti1 C51 117.23(9) . .
O1A Ti1 C51 80.21(9) 3_666 .
O2A Ti1 C51 139.13(9) . .
C31 Ti1 C51 57.22(10) . .
C21 Ti1 C51 57.11(10) . .
C41 Ti1 C51 34.55(10) . .
C11 Ti1 C51 33.94(11) . .
O1A Ti1 Cl1 118.55(6) . .
O1A Ti1 Cl1 88.48(6) 3_666 .
O2A Ti1 Cl1 85.15(6) . .
C31 Ti1 Cl1 134.47(9) . .
C21 Ti1 Cl1 100.71(10) . .
C41 Ti1 Cl1 148.94(8) . .
C11 Ti1 Cl1 91.81(9) . .
C51 Ti1 Cl1 116.24(8) . .
O1A Ti1 Ti1 37.19(5) . 3_666
O1A Ti1 Ti1 35.90(5) 3_666 3_666
O2A Ti1 Ti1 107.12(6) . 3_666
C31 Ti1 Ti1 119.49(9) . 3_666
C21 Ti1 Ti1 150.94(9) . 3_666
C41 Ti1 Ti1 93.15(8) . 3_666
C11 Ti1 Ti1 131.68(8) . 3_666
C51 Ti1 Ti1 99.96(8) . 3_666
Cl1 Ti1 Ti1 106.03(3) . 3_666
C1A O1A Ti1 118.43(15) . .
C1A O1A Ti1 134.54(16) . 3_666
Ti1 O1A Ti1 106.91(8) . 3_666
O1A C1A C2A 108.2(2) . .
O1A C1A H1A1 110.1 . .
C2A C1A H1A1 110.1 . .
O1A C1A H1A2 110.1 . .
C2A C1A H1A2 110.1 . .
H1A1 C1A H1A2 108.4 . .
O2A C2A C1A 106.5(2) . .
O2A C2A H2A1 110.4 . .
C1A C2A H2A1 110.4 . .
O2A C2A H2A2 110.4 . .
C1A C2A H2A2 110.4 . .
H2A1 C2A H2A2 108.6 . .
C3A O2A C2A 113.2(2) . .
C3A O2A Ti1 130.27(18) . .
C2A O2A Ti1 116.55(15) . .
O2A C3A H3A1 109.5 . .
O2A C3A H3A2 109.5 . .
H3A1 C3A H3A2 109.5 . .
O2A C3A H3A3 109.5 . .
H3A1 C3A H3A3 109.5 . .
H3A2 C3A H3A3 109.5 . .
C51 C11 C21 107.3(3) . .
C51 C11 Ti1 73.50(16) . .
C21 C11 Ti1 70.94(17) . .
C51 C11 H11 126.3 . .
C21 C11 H11 126.3 . .
Ti1 C11 H11 121.0 . .
C31 C21 C11 108.0(3) . .
C31 C21 Ti1 72.27(17) . .
C11 C21 Ti1 74.18(18) . .
C31 C21 H21 126.0 . .
C11 C21 H21 126.0 . .
Ti1 C21 H21 119.4 . .
C41 C31 C21 108.3(3) . .
C41 C31 Ti1 73.39(17) . .
C21 C31 Ti1 72.82(18) . .
C41 C31 H31 125.8 . .
C21 C31 H31 125.8 . .
Ti1 C31 H31 119.7 . .
C31 C41 C51 107.7(3) . .
C31 C41 Ti1 71.96(16) . .
C51 C41 Ti1 74.38(16) . .
C31 C41 H41 126.2 . .
C51 C41 H41 126.2 . .
Ti1 C41 H41 119.4 . .
C11 C51 C41 108.7(3) . .
C11 C51 Ti1 72.56(16) . .
C41 C51 Ti1 71.07(15) . .
C11 C51 H51 125.7 . .
C41 C51 H51 125.7 . .
Ti1 C51 H51 122.4 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O1A 1.9848(19) .
Ti1 O1A 2.0460(18) 3_666
Ti1 O2A 2.2027(19) .
Ti1 C31 2.340(3) .
Ti1 C21 2.347(3) .
Ti1 C41 2.358(3) .
Ti1 C11 2.389(3) .
Ti1 C51 2.401(3) .
Ti1 Cl1 2.4032(9) .
Ti1 Ti1 3.2384(14) 3_666
O1A C1A 1.420(3) .
O1A Ti1 2.0460(18) 3_666
C1A C2A 1.511(4) .
C1A H1A1 0.9900 .
C1A H1A2 0.9900 .
C2A O2A 1.445(3) .
C2A H2A1 0.9900 .
C2A H2A2 0.9900 .
O2A C3A 1.429(3) .
C3A H3A1 0.9800 .
C3A H3A2 0.9800 .
C3A H3A3 0.9800 .
C11 C51 1.398(4) .
C11 C21 1.420(4) .
C11 H11 0.9500 .
C21 C31 1.406(5) .
C21 H21 0.9500 .
C31 C41 1.399(4) .
C31 H31 0.9500 .
C41 C51 1.414(4) .
C41 H41 0.9500 .
C51 H51 0.9500 .
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_site_symmetry_1
Ti1 O1A C1A C2A -47.7(3) .
Ti1 O1A C1A C2A 137.1(2) 3_666
O1A C1A C2A O2A 36.3(3) .
C1A C2A O2A C3A 166.5(3) .
C1A C2A O2A Ti1 -14.9(3) .
C51 C11 C21 C31 0.1(3) .
Ti1 C11 C21 C31 -64.9(2) .
C51 C11 C21 Ti1 65.0(2) .
C11 C21 C31 C41 0.8(3) .
Ti1 C21 C31 C41 -65.3(2) .
C11 C21 C31 Ti1 66.1(2) .
C21 C31 C41 C51 -1.4(3) .
Ti1 C31 C41 C51 -66.36(19) .
C21 C31 C41 Ti1 65.0(2) .
C21 C11 C51 C41 -1.0(3) .
Ti1 C11 C51 C41 62.29(19) .
C21 C11 C51 Ti1 -63.3(2) .
C31 C41 C51 C11 1.5(3) .
Ti1 C41 C51 C11 -63.2(2) .
C31 C41 C51 Ti1 64.75(19) .
