Titanium-Oxide Host Clusters with Exchangeable Guests.
Zhang, Guanyun; Li, Wenyun; Liu, Caiyun; Jia, Jiong; Tung, Chen-Ho; Wang, Yifeng; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b10565

data_4126918
_publ_section_title
;
 Titanium-Oxide Host Clusters with Exchangeable Guests.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b10565
_journal_year                    2017
_chemical_formula_moiety
'0.33(C60 Ca2 Cl2 N12 O108 Ti24), 0.33(C30 Ca N6 O54 Ti12), 11.94(Cl1.2), 4(O)'
_chemical_formula_sum            'C30 Ca Cl15 N6 O58 Ti12'
_chemical_formula_weight         2518.99
_chemical_name_systematic
;
 ?
;
_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'
_audit_creation_date             2017-07-23
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_cell_angle_alpha                75.807(3)
_cell_angle_beta                 79.387(3)
_cell_angle_gamma                80.338(3)
_cell_formula_units_Z            3
_cell_length_a                   16.673(5)
_cell_length_b                   22.411(6)
_cell_length_c                   22.543(7)
_cell_measurement_reflns_used    7052
_cell_measurement_temperature    173
_cell_measurement_theta_max      27.821
_cell_measurement_theta_min      1.885
_cell_volume                     7960(4)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.980
_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  0.1195
_diffrn_reflns_av_unetI/netI     0.1674
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            115977
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.821
_diffrn_reflns_theta_min         1.885
_exptl_absorpt_coefficient_mu    1.362
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5950
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0935 before and 0.0783 after correction.
The Ratio of minimum to maximum transmission is 0.7980.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_description       block
_exptl_crystal_F_000             3675
_refine_diff_density_max         3.090
_refine_diff_density_min         -1.427
_refine_diff_density_rms         0.299
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.762
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1443
_refine_ls_number_reflns         37034
_refine_ls_number_restraints     146
_refine_ls_restrained_S_all      1.768
_refine_ls_R_factor_all          0.3053
_refine_ls_R_factor_gt           0.2235
_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/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5560
_refine_ls_wR_factor_ref         0.5814
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16965
_reflns_number_total             37034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10565_si_010.cif
_cod_data_source_block           p-1_sqd
_cod_database_code               4126918
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Restrained distances
 C36-C37
 1.5 with sigma of 0.01
 C37-N7
 1.5 with sigma of 0.01
 C37-C38
 1.5 with sigma of 0.01
 C21-C22
 1.5 with sigma of 0.01
 N6-C22
 1.5 with sigma of 0.01
 C22-C23
 1.5 with sigma of 0.01
 C16-C17
 1.5 with sigma of 0.01
 C18-C17
 1.5 with sigma of 0.01
 C17-N4
 1.5 with sigma of 0.01
 C20-N4
 1.5 with sigma of 0.01
 C26-C27
 1.5 with sigma of 0.01
 C41-C42
 1.5 with sigma of 0.01
 N9-C42
 1.5 with sigma of 0.01
 C1-C2
 1.5 with sigma of 0.01
 N3-C2
 1.5 with sigma of 0.01
 C11-C12
 1.5 with sigma of 0.01
 C12-N1
 1.5 with sigma of 0.01
 C6-C7
 1.5 with sigma of 0.01
 C8-N2
 2.45 with sigma of 0.01
 C9-C10
 1.5 with sigma of 0.01
 C10-N2
 1.5 with sigma of 0.01
 C7-C9
 2.45 with sigma of 0.01
 C8-C10
 2.45 with sigma of 0.01
 C9-N2
 2.45 with sigma of 0.01
 C6-C8
 2.45 with sigma of 0.01
 C8-C9
 1.5 with sigma of 0.01
 N1-C14
 1.5 with sigma of 0.01
 C14-C15
 1.5 with sigma of 0.01
 C15-C13
 1.5 with sigma of 0.01
 C12-C13
 1.5 with sigma of 0.01
 C12-C14
 2.45 with sigma of 0.01
 N1-C15
 2.45 with sigma of 0.01
 C14-C13
 2.45 with sigma of 0.01
 C15-C12
 2.45 with sigma of 0.01
 C42-C44
 2.45 with sigma of 0.01
 C43-C45
 2.45 with sigma of 0.01
 C44-N9
 2.45 with sigma of 0.01
 C45-C42
 2.45 with sigma of 0.01
 C42-C43
 1.5 with sigma of 0.01
 C43-C44
 1.5 with sigma of 0.01
 C44-C45
 1.5 with sigma of 0.01
 N9-C45
 1.5 with sigma of 0.01
 C2-N3
 1.5 with sigma of 0.01
 N3-C5
 1.5 with sigma of 0.01
 C3-C2
 1.5 with sigma of 0.01
 C2-C5
 2.45 with sigma of 0.01
 C3-N3
 2.45 with sigma of 0.01
 C18-N4
 2.45 with sigma of 0.01
 C17-C20
 2.45 with sigma of 0.01
 C23-N6
 2.45 with sigma of 0.01
 C22-C24
 2.45 with sigma of 0.01
 C23-C24
 1.5 with sigma of 0.01
 C19-C20
 1.5 with sigma of 0.01
 C19-C18
 1.5 with sigma of 0.01
 C19-C17
 2.45 with sigma of 0.01
 N4-C19
 2.45 with sigma of 0.01
 C25-C22
 2.45 with sigma of 0.01
 C25-C23
 2.45 with sigma of 0.01
 N6-C25
 1.5 with sigma of 0.01
 C24-C25
 1.5 with sigma of 0.01
 C4-C5
 1.5 with sigma of 0.01
 C3-C4
 1.5 with sigma of 0.01
 N3-C4
 2.45 with sigma of 0.01
 C2-C4
 2.45 with sigma of 0.01
 C39-C37
 2.45 with sigma of 0.01
 C38-C40
 2.45 with sigma of 0.01
 C39-N7
 2.45 with sigma of 0.01
 C40-C37
 2.45 with sigma of 0.01
 C38-C39
 1.5 with sigma of 0.01
 C39-C40
 1.5 with sigma of 0.01
 C40-N7
 1.5 with sigma of 0.01
 C32-N8
 1.5 with sigma of 0.01
 N8-C35
 1.5 with sigma of 0.01
 C35-C34
 1.5 with sigma of 0.01
 C34-C33
 1.5 with sigma of 0.01
 C33-C32
 1.5 with sigma of 0.01
 C32-C35
 2.45 with sigma of 0.01
 N8-C34
 2.45 with sigma of 0.01
 C35-C33
 2.45 with sigma of 0.01
 C34-C32
 2.45 with sigma of 0.01
 C33-N8
 2.45 with sigma of 0.01
 C27-C30
 2.45 with sigma of 0.01
 N5-C29
 2.45 with sigma of 0.01
 C30-C28
 2.45 with sigma of 0.01
 C29-C27
 2.45 with sigma of 0.01
 C28-N5
 2.45 with sigma of 0.01
 C27-N5
 1.5 with sigma of 0.01
 N5-C30
 1.5 with sigma of 0.01
 C30-C29
 1.5 with sigma of 0.01
 C29-C28
 1.5 with sigma of 0.01
 C28-C27
 1.5 with sigma of 0.01
 C31-O72
 1.3 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
N2 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C10: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
N1 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
N9 \\sim C41 \\sim C42 \\sim C43 \\sim C44 \\sim C45: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
N4 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
N6 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
N3 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5: within 1.7A with sigma of 0.01
and sigma for terminal atoms of 0.02
N7 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
N8 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
N5 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: Ca2(0.5) Ca3(0.5) Cl22(0.25) Cl23(0.5) Cl24(0.25) Ca1(0.5)
 Cl30(0.3) Cl31(0.5) Cl32(0.4) Cl25(0.4) Cl27(0.3) Cl20(0.6) Cl21(0.4) Cl4(0.3)
 Cl5(0.7) Cl33(0.45) Cl34(0.55) Cl7(0.5) Cl8(0.4) Cl13(0.65) Cl14(0.35)
 Cl26(0.3) Cl12(0.6) Cl6(0.4) Cl9(0.4) O84(0.5) O85(0.5)
;
_shelx_res_checksum              9772
_shelx_hkl_checksum              42333
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20