The influence of halides in polyoxotitanate cages; dipole moment, splitting and expansion of d-orbitals and electron-electron repulsion.
Hanf, Schirin; Matthews, Peter D.; Li, Ning; Luo, He-Kuan; Wright, Dominic S.; Dalton transactions (Cambridge, England : 2003) 46 (2017) 578–585; doi:10.1039/c6dt04288k

data_7041414
_publ_section_title
;
 The influence of halides in polyoxotitanate cages; dipole moment,
 splitting and expansion of d-orbitals and electron-electron repulsion.
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              578
_journal_page_last               585
_journal_paper_doi               10.1039/c6dt04288k
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C27 H63 Cl O10 Ti3'
_chemical_formula_sum            'C27 H63 Cl O10 Ti3'
_chemical_formula_weight         726.92
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-08-15 deposited with the CCDC.
2016-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.54740(10)
_cell_length_b                   12.54740(10)
_cell_length_c                   49.8245(5)
_cell_measurement_reflns_used    32629
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      1
_cell_volume                     7844.23(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_molecular_graphics    'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.929
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_Laue_measured_fraction_full 0.929
_diffrn_reflns_Laue_measured_fraction_max 0.926
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       59
_diffrn_reflns_limit_l_min       -59
_diffrn_reflns_number            20677
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         25.331
_diffrn_reflns_theta_min         3.652
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.707
_exptl_absorpt_correction_T_max  0.924
_exptl_absorpt_correction_T_min  0.861
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.370
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.27(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         6324
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0975P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1507
_refine_ls_wR_factor_ref         0.1671
_reflns_Friedel_coverage         0.721
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.949
_reflns_number_gt                4224
_reflns_number_total             6324
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt04288k2.cif
_cod_data_source_block           dw1415
_cod_depositor_comments          'Adding full bibliography for 7041414.cif.'
_cod_original_cell_volume        7844.23(15)
_cod_database_code               7041414
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.780
_shelx_estimated_absorpt_t_max   0.901
_shelx_res_checksum              1461