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_4126913
_publ_section_title
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 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         'C18 Cl6 N6 O60 Rb3 Ti12, 11.97(Cl), 9(O)'
_chemical_formula_sum            'C18 Cl18 N6 O79 Rb3 Ti12'
_chemical_formula_weight         3033.55
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_primary     direct
_audit_creation_date             2017-08-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   18.3578(7)
_cell_length_b                   18.3578(7)
_cell_length_c                   62.096(4)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.992
_cell_measurement_theta_min      2.219
_cell_volume                     18123.2(15)
_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)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.0
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.956
_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  0.0637
_diffrn_reflns_av_unetI/netI     0.0558
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       83
_diffrn_reflns_limit_l_min       -80
_diffrn_reflns_number            74110
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.992
_diffrn_reflns_theta_min         0.984
_exptl_absorpt_coefficient_mu    2.441
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6429
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0858 before and 0.0509 after correction.
The Ratio of minimum to maximum transmission is 0.8620.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.668
_exptl_crystal_description       block
_exptl_crystal_F_000             8778
_refine_diff_density_max         3.070
_refine_diff_density_min         -3.349
_refine_diff_density_rms         0.323
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         10265
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1535
_refine_ls_R_factor_gt           0.1242
_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/[\s^2^(Fo^2^)+(0.1561P)^2^+1735.3624P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3546
_refine_ls_wR_factor_ref         0.3685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7274
_reflns_number_total             10265
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10565_si_008.cif
_cod_data_source_block           r-3_sqd
_cod_original_cell_volume        18123.2(19)
_cod_database_code               4126913
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(O21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
2. Others
 Fixed Sof: Cl4(0.5) Cl8(0.5) Cl10(0.825) Cl3(0.5)
;
_shelx_res_checksum              13112
_shelx_hkl_checksum              45747
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20