(TeCl)4(TiCl4) with isolated Te4Cl16 and TiCl4 molecules and second-harmonic-generation
Bonnin, Maxime A.; Beier, Klaus; Bayarjargal, Lkhamsuren; Winkler, Björn; Feldmann, Claus; Dalton Transactions 53 (2024) 4962–4967; doi:10.1039/D4DT00284A

data_7715182
_publ_section_title
;
 (TeCl)4(TiCl4) with isolated Te4Cl16 and TiCl4 molecules and
 second-harmonic-generation
;
_journal_issue                   11
_journal_name_full               'Dalton Transactions'
_journal_page_first              4962
_journal_page_last               4967
_journal_paper_doi               10.1039/D4DT00284A
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '4(Cl3 Te), Cl4 Ti, 4(Cl)'
_chemical_formula_sum            'Cl20 Te4 Ti'
_chemical_formula_weight         1267.30
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_Hall           'I -4'
_space_group_name_H-M_alt        'I -4'
_atom_sites_solution_primary     dual
_audit_creation_date             2023-10-16
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-01-25 deposited with the CCDC.	2024-02-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.1035(15)
_cell_length_b                   12.1035(15)
_cell_length_c                   10.1522(15)
_cell_measurement_reflns_used    4365
_cell_measurement_temperature    210
_cell_measurement_theta_max      29.46
_cell_measurement_theta_min      2.38
_cell_volume                     1487.2(3)
_computing_cell_refinement       'STOE X-Area'
_computing_data_collection       'STOE X-Area'
_computing_data_reduction        'STOE X-Area'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      210
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
 180 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, multiple pinhole'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3863
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.116
_diffrn_reflns_theta_min         2.380
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    5.925
_exptl_absorpt_correction_T_max  0.2179
_exptl_absorpt_correction_T_min  0.1622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.830
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.058
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.076
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.997
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.0211
_refine_ls_R_factor_gt           0.0191
_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^)+(0.0276P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0435
_refine_ls_wR_factor_ref         0.0438
_reflns_d_resolution_high        0.730
_reflns_d_resolution_low         8.558
_reflns_Friedel_coverage         0.840
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.942
_reflns_limit_h_max              15
_reflns_limit_h_min              -16
_reflns_limit_k_max              12
_reflns_limit_k_min              -16
_reflns_limit_l_max              13
_reflns_limit_l_min              -13
_reflns_number_gt                1844
_reflns_number_total             1960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00284a2.cif
_cod_data_source_block           (TeCl4)4(TiCl4)
_cod_depositor_comments          'Adding full bibliography for 7715182.cif.'
_cod_original_cell_volume        1487.2(4)
_cod_database_code               7715182
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.725
_shelx_estimated_absorpt_t_min   0.649
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.50343
 0.49657
;
_shelx_res_checksum              82104
_olex2_submission_special_instructions 'No special instructions were received'