#------------------------------------------------------------------------------
#$Date: 2024-04-05 02:33:24 +0300 (Fri, 05 Apr 2024) $
#$Revision: 290972 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/51/7715182.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7715182
loop_
_publ_author_name
'Bonnin, Maxime A.'
'Beier, Klaus'
'Bayarjargal, Lkhamsuren'
'Winkler, Björn'
'Feldmann, Claus'
_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, ω 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(μ₂-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/[σ²(Fo²)+(0.0276P)²] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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_file
;
TITL kb38_a.res in I-4
    kb38.res
    created by SHELXL-2018/3 at 12:50:34 on 26-Sep-2023
REM Old TITL KB38 in I4 #79
REM SHELXT solution in I-4: R1 0.045, Rweak 0.034, Alpha 0.001
REM <I/s> 0.000 for 0 systematic absences, Orientation as input
REM Flack x = 0.479 ( 0.056 ) from 650 Parsons' quotients
REM Formula found by SHELXT: Ti Cl20 I4
CELL 0.71073 12.1035 12.1035 10.1522 90 90 90
ZERR 2 0.0015 0.0015 0.0015 0 0 0
LATT -2
SYMM -X,-Y,+Z
SYMM +Y,-X,-Z
SYMM -Y,+X,-Z
SFAC Cl Te Ti
UNIT 40 8 2

L.S. 50
PLAN  6
SIZE 0.062 0.08 0.058
TEMP -63.15
CONF
list 4
MORE -1
fmap 2
acta
TWIN -1 0 0 0 -1 0 0 0 -1 2
REM <olex2.extras>
REM <HklSrc "%.\\KB38.hkl">
REM </olex2.extras>

WGHT    0.027600
BASF   0.49657
FVAR       0.14804
TE1   2    0.169373    1.062139    0.852464    11.00000    0.02786    0.02737 =
         0.03025    0.00001    0.00357   -0.00068
TI1   3    0.500000    1.000000    1.250000    10.25000    0.03316    0.03316 =
         0.03417    0.00000    0.00000    0.00000
CL1   1    0.153543    1.055562    1.136339    11.00000    0.03405    0.03903 =
         0.03944   -0.00176   -0.00577   -0.00030
CL2   1    0.243167    1.237901    0.867357    11.00000    0.04777    0.02930 =
         0.06442    0.00031    0.00672   -0.00636
CL5   1    0.358343    0.967729    1.374191    11.00000    0.03689    0.05817 =
         0.04770    0.00372    0.00634   -0.00047
CL3   1    0.338292    0.972798    0.864512    11.00000    0.03393    0.04184 =
         0.05795   -0.00529    0.00213    0.00783
CL4   1    0.162951    1.060380    0.624197    11.00000    0.06612    0.06300 =
         0.03152    0.00083    0.00404    0.00209
HKLF 4




REM  kb38_a.res in I-4
REM wR2 = 0.0438, GooF = S = 0.997, Restrained GooF = 0.997 for all data
REM R1 = 0.0191 for 1844 Fo > 4sig(Fo) and 0.0211 for all 1960 data
REM 58 parameters refined using 0 restraints

END

WGHT      0.0276      0.0000

REM Highest difference peak  0.307,  deepest hole -0.448,  1-sigma level  0.076
Q1    1   0.0846  1.0258  0.8628  11.00000  0.05    0.31
Q2    1   0.1613  1.0683  0.7277  11.00000  0.05    0.30
Q3    1   0.2131  0.9610  0.8606  11.00000  0.05    0.29
Q4    1   0.1675  0.9962  0.9171  11.00000  0.05    0.26
Q5    1   0.2402  1.2032  1.1513  11.00000  0.05    0.26
Q6    1   0.1569  1.0595  1.1899  11.00000  0.05    0.24
;
_shelx_res_checksum              82104
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Te1 Te 0.16937(2) 1.06214(2) 0.85246(3) 0.02849(8) Uani 1 1 d . . . . .
Ti1 Ti 0.500000 1.000000 1.250000 0.0335(4) Uani 1 4 d S T P . .
Cl1 Cl 0.15354(10) 1.05556(11) 1.13634(12) 0.0375(2) Uani 1 1 d . . . . .
Cl2 Cl 0.24317(14) 1.23790(12) 0.8674(2) 0.0472(4) Uani 1 1 d . . . . .
Cl3 Cl 0.33829(11) 0.97280(13) 0.8645(2) 0.0446(3) Uani 1 1 d . . . . .
Cl4 Cl 0.16295(16) 1.06038(15) 0.62420(12) 0.0535(3) Uani 1 1 d . . . . .
Cl5 Cl 0.35834(13) 0.96773(16) 1.37419(18) 0.0476(4) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Te1 0.02786(15) 0.02737(15) 0.03025(12) 0.00001(12) 0.00357(12) -0.00068(11)
Ti1 0.0332(5) 0.0332(5) 0.0342(9) 0.000 0.000 0.000
Cl1 0.0341(6) 0.0390(6) 0.0394(5) -0.0018(7) -0.0058(6) -0.0003(5)
Cl2 0.0478(7) 0.0293(6) 0.0644(12) 0.0003(8) 0.0067(9) -0.0064(5)
Cl3 0.0339(6) 0.0418(6) 0.0580(8) -0.0053(8) 0.0021(8) 0.0078(5)
Cl4 0.0661(12) 0.0630(12) 0.0315(5) 0.0008(6) 0.0040(7) 0.0021(11)
Cl5 0.0369(6) 0.0582(8) 0.0477(9) 0.0037(7) 0.0063(7) -0.0005(6)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl2 Te1 Cl3 94.88(7) . . ?
Cl2 Te1 Cl4 94.98(7) . . ?
Cl3 Te1 Cl4 94.48(7) . . ?
Cl5 Ti1 Cl5 108.72(10) . 2_675 ?
Cl5 Ti1 Cl5 109.85(5) . 8_657 ?
Cl5 Ti1 Cl5 109.85(5) 2_675 8_657 ?
Cl5 Ti1 Cl5 109.85(5) . 7_467 ?
Cl5 Ti1 Cl5 109.85(5) 2_675 7_467 ?
Cl5 Ti1 Cl5 108.72(9) 8_657 7_467 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Te1 Cl2 2.3122(14) . ?
Te1 Cl3 2.3161(13) . ?
Te1 Cl4 2.3188(13) . ?
Ti1 Cl5 2.1638(17) 7_467 ?
Ti1 Cl5 2.1638(17) 8_657 ?
Ti1 Cl5 2.1638(17) 2_675 ?
Ti1 Cl5 2.1638(17) . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.50343
2 0.49657
