A fresnoite-structure-related mixed valent titanium(III/IV) chlorosilicate, Ba3Ti2Si4O14Cl: A flux crystal growth route to Ti(III) containing oxides
Abeysinghe, Dileka; Smith, Mark D.; zur Loye, Hans-Conrad; Journal of Solid State Chemistry 250 (2017) 128–133; doi:10.1016/j.jssc.2017.03.026

data_1560483
_publ_section_title
;
 A fresnoite-structure-related mixed valent titanium(III/IV)
 chlorosilicate, Ba3Ti2Si4O14Cl: A flux crystal growth route to Ti(III)
 containing oxides
;
_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              128
_journal_page_last               133
_journal_paper_doi               10.1016/j.jssc.2017.03.026
_journal_volume                  250
_journal_year                    2017
_chemical_formula_moiety         'Ba3 Cl0.91 O14.09 Si4 Ti2'
_chemical_formula_sum            'Ba3 Cl0.91 O14.09 Si4 Ti2'
_chemical_formula_weight         877.91
_space_group_crystal_system      tetragonal
_space_group_IT_number           127
_space_group_name_Hall           '-P 4 2ab'
_space_group_name_H-M_alt        'P 4/m b m'
_atom_sites_solution_hydrogens   .
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6717(2)
_cell_length_b                   8.6717(2)
_cell_length_c                   18.6492(5)
_cell_measurement_reflns_used    9599
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      36.276
_cell_measurement_theta_min      3.277
_cell_volume                     1402.39(6)
_computing_cell_refinement       'SAINT Version 8.34a (Bruker, 2014)'
_computing_data_collection       'Bruker APEXII v2014.9-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT Version 8.34a (Bruker, 2014)'
_computing_molecular_graphics    various
_computing_publication_material  various
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      300(2)
_diffrn_detector_area_resol_mean 10.4
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_av_unetI/netI     0.0080
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            77293
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        36.445
_diffrn_reflns_theta_max         36.447
_diffrn_reflns_theta_min         2.184
_diffrn_source                   'microfocus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    9.979
_exptl_absorpt_correction_T_max  0.1661
_exptl_absorpt_correction_T_min  0.1117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2014/4 (Bruker, 2014)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    4.158
_exptl_crystal_description       'square plate'
_exptl_crystal_F_000             1585
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.746
_refine_diff_density_min         -1.030
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.00103(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     75
_refine_ls_number_reflns         1895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.215
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0156
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0124P)^2^+1.8036P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0337
_refine_ls_wR_factor_ref         0.0344
_reflns_number_gt                1762
_reflns_number_total             1895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            JSSC-2017-250-128.cif
_cod_data_source_block           da2016b
_cod_original_cell_volume        1402.39(7)
_cod_database_code               1560483
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.435
_shelx_estimated_absorpt_t_max   0.754