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_4126912
_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         '0.5(C8 Cl10 Cs10 N4 O140 S12 Ti24), 5(Cl)'
_chemical_formula_sum            'C4 Cl10 Cs5 N2 O70 S6 Ti12'
_chemical_formula_weight         2982.27
_chemical_name_systematic
;
 ?
;
_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'
_audit_creation_date             2017-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.97(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.37(2)
_cell_length_b                   13.06(2)
_cell_length_c                   24.57(3)
_cell_measurement_reflns_used    1274
_cell_measurement_temperature    173
_cell_measurement_theta_max      26.19
_cell_measurement_theta_min      2.75
_cell_volume                     4600(11)
_computing_cell_refinement       'SAINT V8.30C (?, 2016)'
_computing_data_reduction        'SAINT V8.30C (?, 2016)'
_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 0.948
_diffrn_measured_fraction_theta_max 0.948
_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  0.0480
_diffrn_reflns_av_unetI/netI     0.0998
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            21097
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.381
_diffrn_reflns_theta_min         1.595
_exptl_absorpt_coefficient_mu    3.459
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.4897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.1434 before and 0.0480 after correction. The Ratio of minimum to maximum transmission is 0.6568. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.153
_exptl_crystal_description       block
_exptl_crystal_F_000             2806
_refine_diff_density_max         3.824
_refine_diff_density_min         -5.231
_refine_diff_density_rms         0.372
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         7800
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.1639
_refine_ls_R_factor_gt           0.1199
_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^)+(0.1559P)^2^+270.1184P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3041
_refine_ls_wR_factor_ref         0.3328
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5379
_reflns_number_total             7800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10565_si_013.cif
_cod_data_source_block           p21n
_cod_original_cell_volume        4600(12)
_cod_database_code               4126912
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Restrained distances
 S2-O23
 1.45 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
S2 \\sim O22 \\sim O23 \\sim O25 \\sim O24: within 1.7A with sigma of 0.001 and
sigma for terminal atoms of 0.002
3. Others
 Fixed Sof: Cl5(0.5) Cl6(0.5)
;
_shelx_res_checksum              26617
_shelx_hkl_checksum              25797
_olex2_submission_special_instructions 'No special instructions were received'