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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/4/34/53/4345307.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_4345307
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         'C18 H46 Cl4 In2 O12'
_chemical_formula_sum            'C18 H46 Cl4 In2 O12'
_chemical_formula_weight         825.99
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90.66(3)
_cell_angle_beta                 110.30(4)
_cell_angle_gamma                112.72(3)
_cell_formula_units_Z            1
_cell_length_a                   8.848(3)
_cell_length_b                   9.437(3)
_cell_length_c                   10.924(4)
_cell_measurement_reflns_used    6369
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.6900
_cell_measurement_theta_min      2.8390
_cell_volume                     777.9(6)
_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      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.612
_diffrn_measurement_device_type  'PX Xcalibur'
_diffrn_measurement_method       'ω and φ'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.612
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9345
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.612
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         36.775
_diffrn_reflns_theta_min         2.845
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.877
_exptl_absorpt_correction_T_max  0.885
_exptl_absorpt_correction_T_min  0.663
_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            colorless
_exptl_crystal_density_diffrn    1.763
_exptl_crystal_description       needle
_exptl_crystal_F_000             416
_exptl_crystal_size_max          0.324
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.092
_refine_diff_density_max         1.011
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.167
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         4759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0392
_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)+(0.0545P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0957
_refine_ls_wR_factor_ref         0.0975
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4082
_reflns_number_total             4759
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b02824_si_001.cif
_cod_data_source_block           9
_cod_original_cell_volume        777.9(5)
_cod_database_code               4345307
_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   0.582
_shelx_estimated_absorpt_t_max   0.846
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
In1 In 0.59926(3) 0.40635(3) 0.61250(2) 0.01249(7) Uani 1 1 d . . . . .
Cl1 Cl 0.49485(11) 0.23724(10) 0.75935(8) 0.01963(17) Uani 1 1 d . . . . .
Cl2 Cl 0.87757(11) 0.38404(11) 0.66572(10) 0.02438(19) Uani 1 1 d . . . . .
O1A O 0.3571(3) 0.4344(3) 0.5225(2) 0.0140(4) Uani 1 1 d . . . . .
C1A C 0.1941(4) 0.3489(4) 0.5357(3) 0.0160(6) Uani 1 1 d . . . . .
H1A1 H 0.1382 0.4205 0.5408 0.019 Uiso 1 1 calc R U . . .
H1A2 H 0.2178 0.3076 0.6199 0.019 Uiso 1 1 calc R U . . .
C2A C 0.0661(4) 0.2155(4) 0.4238(3) 0.0181(7) Uani 1 1 d . . . . .
H2A1 H -0.0491 0.1678 0.4342 0.022 Uiso 1 1 calc R U . . .
H2A2 H 0.0460 0.2548 0.3386 0.022 Uiso 1 1 calc R U . . .
O2A O 0.1341(3) 0.1000(3) 0.4224(2) 0.0174(5) Uani 1 1 d . . . . .
C3A C 0.0212(5) -0.0227(4) 0.3105(4) 0.0224(7) Uani 1 1 d . . . . .
H3A1 H -0.1001 -0.0660 0.3082 0.034 Uiso 1 1 calc R U . . .
H3A2 H 0.0641 -0.1049 0.3180 0.034 Uiso 1 1 calc R U . . .
H3A3 H 0.0223 0.0190 0.2289 0.034 Uiso 1 1 calc R U . . .
O1B O 0.4605(3) 0.2130(3) 0.4399(2) 0.0157(4) Uani 1 1 d . . . . .
H1B H 0.3507 0.1678 0.4208 0.024 Uiso 1 1 calc R U . . .
C1B C 0.5139(5) 0.1212(4) 0.3741(4) 0.0206(7) Uani 1 1 d . . . . .
H1B1 H 0.4080 0.0324 0.3120 0.025 Uiso 1 1 calc R U . . .
H1B2 H 0.5873 0.0790 0.4399 0.025 Uiso 1 1 calc R U . . .
C2B C 0.6181(5) 0.2185(4) 0.2995(4) 0.0233(7) Uani 1 1 d . . . . .
H2B1 H 0.7235 0.3079 0.3613 0.028 Uiso 1 1 calc R U . . .
H2B2 H 0.6592 0.1554 0.2570 0.028 Uiso 1 1 calc R U . . .
O2B O 0.5098(4) 0.2735(3) 0.2013(3) 0.0265(6) Uani 1 1 d . . . . .
C3B C 0.6054(6) 0.3673(5) 0.1267(4) 0.0368(10) Uani 1 1 d . . . . .
H3B1 H 0.7094 0.4570 0.1868 0.055 Uiso 1 1 calc R U . . .
H3B2 H 0.5281 0.4042 0.0603 0.055 Uiso 1 1 calc R U . . .
H3B3 H 0.6436 0.3047 0.0824 0.055 Uiso 1 1 calc R U . . .
O1C O 0.7191(4) 0.6142(3) 0.7740(2) 0.0215(5) Uani 1 1 d . . . . .
H1C H 0.6722 0.6726 0.7860 0.032 Uiso 1 1 calc R U . A 1
C1C C 0.8403(14) 0.6020(14) 0.9051(13) 0.021(2) Uani 0.502(9) 1 d . . P B 1
H1C1 H 0.7696 0.5532 0.9585 0.025 Uiso 0.502(9) 1 calc R U P B 1
H1C2 H 0.8948 0.5329 0.8901 0.025 Uiso 0.502(9) 1 calc R U P B 1
C2C C 0.9841(10) 0.7557(11) 0.9818(8) 0.0178(16) Uani 0.502(9) 1 d . . P B 1
H2C1 H 0.9322 0.8308 0.9861 0.021 Uiso 0.502(9) 1 calc R U P B 1
H2C2 H 1.0449 0.7436 1.0734 0.021 Uiso 0.502(9) 1 calc R U P B 1
O2C O 1.1079(6) 0.8132(6) 0.9202(5) 0.0218(15) Uani 0.502(9) 1 d . . P B 1
C4C C 0.7934(15) 0.6132(15) 0.9134(12) 0.019(2) Uani 0.498(9) 1 d . . P B 2
H4C1 H 0.7574 0.5049 0.9312 0.023 Uiso 0.498(9) 1 calc R U P B 2
H4C2 H 0.7525 0.6697 0.9625 0.023 Uiso 0.498(9) 1 calc R U P B 2
C5C C 0.9889(11) 0.6920(10) 0.9546(8) 0.0194(17) Uani 0.498(9) 1 d . . P B 2
H5C1 H 1.0466 0.6665 1.0413 0.023 Uiso 0.498(9) 1 calc R U P B 2
H5C2 H 1.0242 0.6534 0.8891 0.023 Uiso 0.498(9) 1 calc R U P B 2
O3C O 1.0472(7) 0.8557(6) 0.9648(5) 0.0211(15) Uani 0.498(9) 1 d . . P B 2
C3C C 1.2409(5) 0.9456(5) 0.9913(4) 0.0324(9) Uani 1 1 d . . . . .
H3C1 H 1.3145 0.9242 1.0727 0.049 Uiso 1 1 calc R U . B 1
H3C2 H 1.1938 1.0162 1.0139 0.049 Uiso 1 1 calc R U . B 1
H3C3 H 1.3128 0.9944 0.9398 0.049 Uiso 1 1 calc R U . B 1
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'
In In -0.7276 1.3100 '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 In1 O1A 73.79(9) 2_666 .
O1A In1 O1B 87.90(9) 2_666 .
O1A In1 O1B 80.60(10) . .
O1A In1 O1C 88.14(9) 2_666 .
O1A In1 O1C 93.34(10) . .
O1B In1 O1C 173.49(9) . .
O1A In1 Cl2 95.02(7) 2_666 .
O1A In1 Cl2 166.94(6) . .
O1B In1 Cl2 92.49(8) . .
O1C In1 Cl2 93.00(9) . .
O1A In1 Cl1 167.71(6) 2_666 .
O1A In1 Cl1 94.31(7) . .
O1B In1 Cl1 93.25(7) . .
O1C In1 Cl1 89.53(7) . .
Cl2 In1 Cl1 97.15(4) . .
C1A O1A In1 126.4(2) . 2_666
C1A O1A In1 126.84(19) . .
In1 O1A In1 106.21(9) 2_666 .
O1A C1A C2A 113.7(3) . .
O1A C1A H1A1 108.8 . .
C2A C1A H1A1 108.8 . .
O1A C1A H1A2 108.8 . .
C2A C1A H1A2 108.8 . .
H1A1 C1A H1A2 107.7 . .
O2A C2A C1A 110.5(3) . .
O2A C2A H2A1 109.5 . .
C1A C2A H2A1 109.5 . .
O2A C2A H2A2 109.5 . .
C1A C2A H2A2 109.5 . .
H2A1 C2A H2A2 108.1 . .
C3A O2A C2A 111.7(3) . .
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 . .
C1B O1B In1 135.0(2) . .
C1B O1B H1B 109.5 . .
In1 O1B H1B 113.3 . .
O1B C1B C2B 110.0(3) . .
O1B C1B H1B1 109.7 . .
C2B C1B H1B1 109.7 . .
O1B C1B H1B2 109.7 . .
C2B C1B H1B2 109.7 . .
H1B1 C1B H1B2 108.2 . .
O2B C2B C1B 109.5(3) . .
O2B C2B H2B1 109.8 . .
C1B C2B H2B1 109.8 . .
O2B C2B H2B2 109.8 . .
C1B C2B H2B2 109.8 . .
H2B1 C2B H2B2 108.2 . .
C2B O2B C3B 111.2(3) . .
O2B C3B H3B1 109.5 . .
O2B C3B H3B2 109.5 . .
H3B1 C3B H3B2 109.5 . .
O2B C3B H3B3 109.5 . .
H3B1 C3B H3B3 109.5 . .
H3B2 C3B H3B3 109.5 . .
C4C O1C In1 125.3(5) . .
C1C O1C In1 115.5(5) . .
C1C O1C H1C 109.5 . .
In1 O1C H1C 127.4 . .
C2C C1C O1C 113.3(9) . .
C2C C1C H1C1 108.9 . .
O1C C1C H1C1 108.9 . .
C2C C1C H1C2 108.9 . .
O1C C1C H1C2 108.9 . .
H1C1 C1C H1C2 107.7 . .
O2C C2C C1C 109.9(8) . .
O2C C2C H2C1 109.7 . .
C1C C2C H2C1 109.7 . .
O2C C2C H2C2 109.7 . .
C1C C2C H2C2 109.7 . .
H2C1 C2C H2C2 108.2 . .
C3C O2C C2C 110.4(6) . .
O1C C4C C5C 106.4(8) . .
O1C C4C H4C1 110.4 . .
C5C C4C H4C1 110.4 . .
O1C C4C H4C2 110.4 . .
C5C C4C H4C2 110.4 . .
H4C1 C4C H4C2 108.6 . .
O3C C5C C4C 111.0(8) . .
O3C C5C H5C1 109.4 . .
C4C C5C H5C1 109.4 . .
O3C C5C H5C2 109.4 . .
C4C C5C H5C2 109.4 . .
H5C1 C5C H5C2 108.0 . .
C5C O3C C3C 115.3(6) . .
O2C C3C H3C1 109.5 . .
O2C C3C H3C2 109.5 . .
H3C1 C3C H3C2 109.5 . .
O2C C3C H3C3 109.5 . .
H3C1 C3C H3C3 109.5 . .
H3C2 C3C H3C3 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
In1 O1A 2.140(2) 2_666
In1 O1A 2.147(2) .
In1 O1B 2.230(3) .
In1 O1C 2.259(3) .
In1 Cl2 2.4199(12) .
In1 Cl1 2.4336(12) .
O1A C1A 1.414(3) .
O1A In1 2.140(2) 2_666
C1A C2A 1.505(5) .
C1A H1A1 0.9900 .
C1A H1A2 0.9900 .
C2A O2A 1.436(4) .
C2A H2A1 0.9900 .
C2A H2A2 0.9900 .
O2A C3A 1.435(4) .
C3A H3A1 0.9800 .
C3A H3A2 0.9800 .
C3A H3A3 0.9800 .
O1B C1B 1.424(4) .
O1B H1B 0.8400 .
C1B C2B 1.497(5) .
C1B H1B1 0.9900 .
C1B H1B2 0.9900 .
C2B O2B 1.422(5) .
C2B H2B1 0.9900 .
C2B H2B2 0.9900 .
O2B C3B 1.442(4) .
C3B H3B1 0.9800 .
C3B H3B2 0.9800 .
C3B H3B3 0.9800 .
O1C C4C 1.436(13) .
O1C C1C 1.500(14) .
O1C H1C 0.8400 .
C1C C2C 1.494(14) .
C1C H1C1 0.9900 .
C1C H1C2 0.9900 .
C2C O2C 1.417(10) .
C2C H2C1 0.9900 .
C2C H2C2 0.9900 .
O2C C3C 1.326(6) .
C4C C5C 1.485(14) .
C4C H4C1 0.9900 .
C4C H4C2 0.9900 .
C5C O3C 1.416(10) .
C5C H5C1 0.9900 .
C5C H5C2 0.9900 .
O3C C3C 1.506(7) .
C3C H3C1 0.9800 .
C3C H3C2 0.9800 .
C3C H3C3 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
_geom_hbond_site_symmetry_A
C1A H1A2 Cl1 0.99 2.73 3.446(4) 129.5 .
C3A H3A3 O2C 0.98 2.58 3.380(6) 138.9 2_666
C3A H3A3 O3C 0.98 2.44 3.388(7) 161.6 2_666
O1B H1B O2A 0.84 1.78 2.598(3) 164.6 .
O1C H1C O2B 0.84 1.91 2.707(4) 157.4 2_666
C1C H1C2 Cl2 0.99 2.74 3.489(12) 133.0 .
C4C H4C1 Cl1 0.99 2.76 3.455(13) 127.4 .
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
In1 O1A C1A C2A 73.6(3) 2_666
In1 O1A C1A C2A -96.9(3) .
O1A C1A C2A O2A 65.1(3) .
C1A C2A O2A C3A -175.4(2) .
In1 O1B C1B C2B -70.6(4) .
O1B C1B C2B O2B -61.8(4) .
C1B C2B O2B C3B -179.8(3) .
In1 O1C C1C C2C 149.3(6) .
O1C C1C C2C O2C -70.3(10) .
C1C C2C O2C C3C -176.7(7) .
In1 O1C C4C C5C 104.9(8) .
O1C C4C C5C O3C 76.4(10) .
C4C C5C O3C C3C -173.5(7) .
