#------------------------------------------------------------------------------
#$Date: 2019-11-23 09:43:15 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232762 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/81/4348116.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_4348116
loop_
_publ_author_name
'Hou, Jie'
'Hu, Junyi'
'Sun, Qing'
'Zhang, Guanyun'
'Tung, Chen-Ho'
'Wang, Yifeng'
_publ_section_title
;
 A Post-Functionalizable Iso-Polyoxotitanate Cage Cluster.
;
_journal_issue                   14
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7075
_journal_page_last               7078
_journal_paper_doi               10.1021/acs.inorgchem.6b00982
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         '3(I), C33 O11 Ti3'
_chemical_formula_sum            'C33 I3 O11 Ti3'
_chemical_formula_weight         1096.73
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_primary     heavy
_audit_creation_date             2015-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   13.102(2)
_cell_length_b                   13.102(2)
_cell_length_c                   49.573(16)
_cell_measurement_reflns_used    1664
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      23.03
_cell_measurement_theta_min      2.43
_cell_volume                     7370(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0233
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            8061
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.463
_diffrn_reflns_theta_min         2.434
_exptl_absorpt_coefficient_mu    2.402
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       block
_exptl_crystal_F_000             3066
_refine_diff_density_max         1.836
_refine_diff_density_min         -2.214
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     85
_refine_ls_number_reflns         1873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.1395
_refine_ls_R_factor_gt           0.1035
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1521P)²+96.9043P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3112
_refine_ls_wR_factor_ref         0.3512
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1203
_reflns_number_total             1873
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic6b00982_si_001.cif
_cod_data_source_block           r-3c
_cod_original_cell_volume        7369(3)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4348116
_shelxl_version_number           2013-4
_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.
;
_olex2_refinement_description
;
1. Others
 Fixed Sof: C1(0.5) C6(0.66667)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'y, x, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'y+2/3, x+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'y+1/3, x+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-y, -x, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-y+2/3, -x+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
'-y+1/3, -x+2/3, z+1/6'
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
I2 I -0.6667 -0.3333 0.72676(8) 0.2176(19) Uani 1 3 d S T P
I1 I -0.6667 -0.3333 0.6667 0.194(2) Uani 1 6 d S T P
Ti1 Ti -0.3333 0.19906(14) 0.5833 0.0776(9) Uani 1 2 d S T P
O2 O -0.3333 0.3333 0.55946(15) 0.0521(18) Uani 1 3 d S T P
O3 O -0.3353(10) 0.1129(6) 0.61078(12) 0.130(4) Uani 1 1 d . . .
O1 O -0.1666(6) 0.3333 0.5833 0.100(3) Uani 1 2 d S T P
C1 C -0.0329(14) 0.3900(16) 0.5853(3) 0.075(4) Uani 0.5 1 d . . .
C3 C -0.355(3) 0.0105(17) 0.6246(3) 0.216(12) Uani 1 1 d . . .
C1AA C -0.4025(19) 0.0009(15) 0.6508(3) 0.171(7) Uani 1 1 d . . .
C5 C -0.3333 0.3333 0.5306(2) 0.092(5) Uani 1 3 d S T P
C4 C -0.256(3) -0.010(2) 0.6202(4) 0.248(14) Uani 1 1 d . . .
C2 C -0.0165(15) 0.3276(17) 0.6096(4) 0.174(7) Uani 1 1 d . . .
C6 C -0.413(3) 0.257(3) 0.5139(11) 0.27(2) Uani 0.6667 1 d . . .
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'
I I -0.4742 1.8119 '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'
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
I2 I1 I2 180.0 . 25_346
Ti1 Ti1 Ti1 60.001(1) 3_455 2_565
O2 Ti1 Ti1 44.06(12) 16 2_565
O2 Ti1 Ti1 44.06(11) . 3_455
O2 Ti1 Ti1 44.06(12) . 2_565
O2 Ti1 Ti1 44.06(11) 16 3_455
O2 Ti1 O2 67.9(3) . 16
O3 Ti1 Ti1 122.9(3) 17_445 2_565
O3 Ti1 Ti1 123.8(3) . 2_565
O3 Ti1 Ti1 122.9(3) . 3_455
O3 Ti1 Ti1 123.8(3) 17_445 3_455
O3 Ti1 O2 163.3(3) 17_445 16
O3 Ti1 O2 95.4(3) 17_445 .
O3 Ti1 O2 95.5(3) . 16
O3 Ti1 O2 163.3(3) . .
O3 Ti1 O3 101.3(4) 17_445 .
O3 Ti1 O1 102.9(4) 17_445 3_455
O3 Ti1 O1 102.9(4) . .
O3 Ti1 O1 101.5(4) 17_445 .
O3 Ti1 O1 101.5(4) . 3_455
O1 Ti1 Ti1 40.59(17) . 2_565
O1 Ti1 Ti1 100.59(17) . 3_455
O1 Ti1 Ti1 40.59(17) 3_455 3_455
O1 Ti1 Ti1 100.59(17) 3_455 2_565
O1 Ti1 O2 73.99(14) 3_455 .
O1 Ti1 O2 73.99(14) . .
O1 Ti1 O2 73.99(14) . 16
O1 Ti1 O2 74.00(14) 3_455 16
O1 Ti1 O1 141.2(3) . 3_455
Ti1 O2 Ti1 91.9(2) . 3_455
Ti1 O2 Ti1 91.9(2) 2_565 3_455
Ti1 O2 Ti1 91.9(2) . 2_565
C5 O2 Ti1 123.93(16) . .
C5 O2 Ti1 123.93(16) . 3_455
C5 O2 Ti1 123.93(17) . 2_565
C3 O3 Ti1 157.3(10) . .
Ti1 O1 Ti1 98.8(3) . 2_565
C1 O1 Ti1 155.3(7) 16 2_565
C1 O1 Ti1 105.6(7) 16 .
C1 O1 Ti1 155.3(7) . .
C1 O1 Ti1 105.6(7) . 2_565
C1 O1 C1 50.5(14) 16 .
O1 C1 C2 103.0(12) . .
O1 C1 C2 98.0(11) . 16
C1 C1 O1 64.8(7) 16 .
C1 C1 C2 61.4(14) 16 16
C1 C1 C2 70.3(15) 16 .
C2 C1 C2 110.8(16) . 16
O3 C3 C1AA 113.1(13) . .
O3 C3 C4 110.2(18) . .
C1AA C3 C4 120.5(17) . .
C6 C5 O2 129(2) 2_565 .
C6 C5 O2 129(2) 3_455 .
C6 C5 O2 129(2) . .
C6 C5 C6 85(4) . 2_565
C6 C5 C6 85(4) 2_565 3_455
C6 C5 C6 85(4) . 3_455
C1 C2 C1 48.4(13) . 16
C5 C6 C6 47.7(18) . 3_455
C5 C6 C6 47.7(18) . 2_565
C6 C6 C6 59.999(18) 3_455 2_565
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
I2 I1 2.979(4) .
I1 I2 2.979(4) 25_346
Ti1 Ti1 3.047(3) 2_565
Ti1 Ti1 3.047(3) 3_455
Ti1 O2 2.120(4) 16
Ti1 O2 2.120(4) .
Ti1 O3 1.760(6) 17_445
Ti1 O3 1.760(6) .
Ti1 O1 2.006(5) 3_455
Ti1 O1 2.006(5) .
O2 Ti1 2.120(4) 3_455
O2 Ti1 2.120(4) 2_565
O2 C5 1.430(14) .
O3 C3 1.410(13) .
O1 Ti1 2.006(5) 2_565
O1 C1 1.526(17) .
O1 C1 1.526(17) 16
C1 C1 1.30(4) 16
C1 C2 1.53(2) .
C1 C2 1.64(2) 16
C3 C1AA 1.42(2) .
C3 C4 1.47(3) .
C5 C6 1.31(3) 2_565
C5 C6 1.31(3) .
C5 C6 1.31(3) 3_455
C2 C1 1.64(2) 16
C6 C6 1.76(5) 2_565
C6 C6 1.76(5) 3_455
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
_geom_torsion_site_symmetry_4
Ti1 Ti1 O3 C3 120(3) 3_455 .
Ti1 Ti1 O3 C3 -166(3) 2_565 .
Ti1 O2 C5 C6 -178(2) . 3_455
Ti1 O2 C5 C6 62(2) 2_565 2_565
Ti1 O2 C5 C6 62(2) 3_455 3_455
Ti1 O2 C5 C6 62(2) . .
Ti1 O2 C5 C6 -178(2) 3_455 2_565
Ti1 O2 C5 C6 -178(2) 2_565 .
Ti1 O2 C5 C6 -58(2) 2_565 3_455
Ti1 O2 C5 C6 -58(2) 3_455 .
Ti1 O2 C5 C6 -58(2) . 2_565
Ti1 O3 C3 C1AA -139(2) . .
Ti1 O3 C3 C4 83(4) . .
Ti1 O1 C1 C1 -173.1(12) 2_565 16
Ti1 O1 C1 C1 16(3) . 16
Ti1 O1 C1 C2 126.4(11) 2_565 .
Ti1 O1 C1 C2 69.2(19) . 16
Ti1 O1 C1 C2 -120.1(10) 2_565 16
Ti1 O1 C1 C2 -44(2) . .
O2 Ti1 O3 C3 155(3) . .
O2 Ti1 O3 C3 157(3) 16 .
O2 C5 C6 C6 -137.5(15) . 2_565
O2 C5 C6 C6 137.5(15) . 3_455
O3 Ti1 O3 C3 -23(3) 17_445 .
O1 Ti1 O3 C3 83(3) 3_455 .
O1 Ti1 O3 C3 -128(3) . .
O1 C1 C2 C1 56.8(10) . 16
C1 O1 C1 C2 -60.6(14) 16 .
C1 O1 C1 C2 53.0(13) 16 16
C2 C1 C2 C1 -47.1(14) 16 16
C6 C5 C6 C6 85(3) 3_455 2_565
C6 C5 C6 C6 -85(3) 2_565 3_455
