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_4126916
_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         'C24 Cl4 Cs3 N6 O60 Ti12, 14.67(Cl), 9(O)'
_chemical_formula_sum            'C24 Cl18.66 Cs3 N6 O69 Ti12'
_chemical_formula_weight         3111.50
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2017-08-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.6260(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.9221(10)
_cell_length_b                   23.0542(15)
_cell_length_c                   17.7342(12)
_cell_measurement_reflns_used    8634
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.767
_cell_measurement_theta_min      2.30
_cell_volume                     5654.0(7)
_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)'
_computing_structure_solution    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.990
_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  0.0353
_diffrn_reflns_av_unetI/netI     0.0756
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            40971
_diffrn_reflns_point_group_measured_fraction_full 0.918
_diffrn_reflns_point_group_measured_fraction_max 0.892
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.633
_diffrn_reflns_theta_min         1.973
_exptl_absorpt_coefficient_mu    2.283
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6550
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_description       block
_exptl_crystal_F_000             2969
_refine_diff_density_max         7.903
_refine_diff_density_min         -2.801
_refine_diff_density_rms         0.257
_refine_ls_abs_structure_details
;
 Flack x determined using 6504 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.040(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1107
_refine_ls_number_reflns         23469
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.1125
_refine_ls_R_factor_gt           0.0866
_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^)+(0.1700P)^2^+38.4431P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2441
_refine_ls_wR_factor_ref         0.2713
_reflns_Friedel_coverage         0.759
_reflns_Friedel_fraction_full    0.834
_reflns_Friedel_fraction_max     0.789
_reflns_number_gt                17713
_reflns_number_total             23469
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b10565_si_003.cif
_cod_data_source_block           p21
_cod_database_code               4126916
_shelxl_version_number           2013-4
_olex2_refinement_description
;
1. Restrained distances
 C19-C20
 1.5 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
O58 \\sim N5 \\sim C17 \\sim C18 \\sim C19 \\sim C20: within 1.7A with sigma of
0.01 and sigma for terminal atoms of 0.02
3. Others
 Fixed Sof: Cl15(0.75) Cl20(0.25) Cl9(0.6667)
;
_shelx_res_checksum              75864
_shelx_hkl_checksum              33676
_olex2_submission_special_instructions 'No special instructions were received'