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_4126911
_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
'C16.2 Cl2 K2.5 N6 O58.5 Ti12, 14(Cl), 2(C0.4 O0.25), C O, 6(O)'
_chemical_formula_sum            'C18 Cl22 K2.5 N6 O76 Ti12'
_chemical_formula_weight         2968.69
_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             2017-07-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.30 svn.r3356 for OlexSys, GUI svn.r5269)
;
_cell_angle_alpha                68.4080(10)
_cell_angle_beta                 74.8360(10)
_cell_angle_gamma                85.0850(10)
_cell_formula_units_Z            1
_cell_length_a                   11.6472(9)
_cell_length_b                   14.8259(12)
_cell_length_c                   16.4433(13)
_cell_measurement_reflns_used    4584
_cell_measurement_temperature    173
_cell_measurement_theta_max      24.061
_cell_measurement_theta_min      1.375
_cell_volume                     2548.1(3)
_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 0.875
_diffrn_measured_fraction_theta_max 0.999
_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  0.0655
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 0.875
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            35652
_diffrn_reflns_point_group_measured_fraction_full 0.875
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.061
_diffrn_reflns_theta_max         24.061
_diffrn_reflns_theta_min         1.375
_exptl_absorpt_coefficient_mu    1.674
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6190
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0793 before and 0.0523 after correction.
The Ratio of minimum to maximum transmission is 0.8309.
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    1.935
_exptl_crystal_description       block
_exptl_crystal_F_000             1444
_refine_diff_density_max         2.906
_refine_diff_density_min         -1.352
_refine_diff_density_rms         0.236
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         8057
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.130
_refine_ls_R_factor_all          0.1383
_refine_ls_R_factor_gt           0.1166
_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^)+(0.0845P)^2^+89.5359P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2855
_refine_ls_wR_factor_ref         0.2967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6304
_reflns_number_total             8057
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10565_si_009.cif
_cod_data_source_block           p-1_sqd
_cod_original_formula_sum        'C18 Cl22 K2.50 N6 O76 Ti12'
_cod_database_code               4126911
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Restrained distances
 C6-C4
 1.45 with sigma of 0.02
 C5-C4
 1.45 with sigma of 0.02
 C4-O29
 2.35 with sigma of 0.02
 O28-C4
 2.35 with sigma of 0.02
 C1-C11
 1.45 with sigma of 0.02
 C1-O30
 2.35 with sigma of 0.02
 C1-C2
 1.45 with sigma of 0.02
 O30-C2
 1.45 with sigma of 0.02
2. Others
 Fixed Sof: K2(0.25) O28(0.75) O31(0.5) C5(0.6) C9(0.5) O29(0.25) C6(0.4)
 O32(0.5) C8(0.5)
;
_shelx_res_checksum              76905
_shelx_hkl_checksum              68297
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20