#------------------------------------------------------------------------------
#$Date: 2024-11-09 04:04:16 +0200 (Sat, 09 Nov 2024) $
#$Revision: 295849 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/95/7249559.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_7249559
loop_
_publ_author_name
'Singh, Puspendra'
'Khan, Mariya'
'Duthie, Andrew'
'Butcher, Ray J.'
_publ_section_title
;
 Synthesis and characterization of carbonyl functionalized
 organotellurium(iv) derivatives
;
_journal_issue                   48
_journal_name_full               'RSC Advances'
_journal_page_first              35650
_journal_page_last               35656
_journal_paper_doi               10.1039/D4RA06023G
_journal_volume                  14
_journal_year                    2024
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C14 H18 Cl2 O2 Te'
_chemical_formula_sum            'C14 H18 Cl2 O2 Te'
_chemical_formula_weight         416.78
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-08-18 deposited with the CCDC.	2024-10-29 downloaded from the CCDC.
;
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 116.320(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            2
_cell_length_a                   8.389(5)
_cell_length_b                   12.312(5)
_cell_length_c                   8.461(5)
_cell_measurement_reflns_used    6202
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      41.0655
_cell_measurement_theta_min      2.6813
_cell_volume                     783.3(7)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'Sir92 Altomare et al. 1993)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.6501
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0523
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            11130
_diffrn_reflns_point_group_measured_fraction_full 0.813
_diffrn_reflns_point_group_measured_fraction_max 0.708
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         41.134
_diffrn_reflns_theta_min         2.686
_exptl_absorpt_coefficient_mu    2.235
_exptl_absorpt_correction_T_max  0.733
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_description       prism
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.4405
_exptl_crystal_size_mid          0.2723
_exptl_crystal_size_min          0.2324
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.985
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.025(16)
_refine_ls_extinction_coef       0.0116(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     179
_refine_ls_number_reflns         7370
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0292
_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)+(0.0131P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0569
_refine_ls_wR_factor_ref         0.0601
_reflns_Friedel_coverage         0.410
_reflns_Friedel_fraction_full    0.611
_reflns_Friedel_fraction_max     0.425
_reflns_number_gt                6779
_reflns_number_total             7370
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4ra06023g2.cif
_cod_data_source_block           mk46
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7249559
_shelx_shelxl_version_number     2019/3
_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.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
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
Te Te 0.59236(2) 0.60750(2) 0.36522(2) 0.01220(4) Uani 1 1 d . . . . .
Cl1 Cl 0.90049(9) 0.57228(6) 0.39084(9) 0.01921(12) Uani 1 1 d . . . . .
Cl2 Cl 0.29189(8) 0.62117(8) 0.35212(8) 0.02132(16) Uani 1 1 d . . . . .
O2 O 0.6029(4) 0.28098(18) -0.0295(3) 0.0258(5) Uani 1 1 d . . . . .
H2 H 0.558319 0.340272 -0.019998 0.072(19) Uiso 1 1 calc R . . . .
O1 O 0.5083(3) 0.42944(18) 0.1118(3) 0.0215(4) Uani 1 1 d . . . . .
C11 C 0.5992(4) 0.3837(2) 0.2580(3) 0.0150(4) Uani 1 1 d . . . . .
C12 C 0.6934(4) 0.2862(2) 0.2756(3) 0.0158(4) Uani 1 1 d . . . . .
H12 H 0.757460 0.254101 0.388480 0.019 Uiso 1 1 calc R U . . .
C1 C 0.7096(3) 0.6841(2) 0.6165(3) 0.0131(4) Uani 1 1 d . . . . .
C2 C 0.7047(3) 0.6432(2) 0.7694(3) 0.0149(4) Uani 1 1 d . . . . .
C3 C 0.7919(4) 0.7037(2) 0.9243(4) 0.0192(5) Uani 1 1 d . . . . .
H3 H 0.793279 0.676818 1.030154 0.023 Uiso 1 1 calc R U . . .
C6 C 0.7904(4) 0.7841(2) 0.6163(3) 0.0148(4) Uani 1 1 d . . . . .
C10 C 0.6011(4) 0.4372(2) 0.4196(4) 0.0172(5) Uani 1 1 d . . . . .
H10A H 0.710686 0.418238 0.526527 0.021 Uiso 1 1 calc R U . . .
H10B H 0.496541 0.414761 0.436834 0.021 Uiso 1 1 calc R U . . .
C9 C 0.7892(4) 0.8343(2) 0.4529(4) 0.0199(5) Uani 1 1 d . . . . .
H9A H 0.824369 0.910749 0.475678 0.030 Uiso 1 1 calc R U . . .
H9B H 0.669302 0.829269 0.355298 0.030 Uiso 1 1 calc R U . . .
H9C H 0.873077 0.795348 0.421579 0.030 Uiso 1 1 calc R U . . .
C8 C 0.9684(5) 0.8641(3) 1.0994(4) 0.0289(7) Uani 1 1 d . . . . .
H8A H 1.073661 0.823909 1.181064 0.043 Uiso 1 1 calc R U . . .
H8B H 0.886621 0.873769 1.152510 0.043 Uiso 1 1 calc R U . . .
H8C H 1.004729 0.935349 1.075094 0.043 Uiso 1 1 calc R U . . .
C13 C 0.6924(4) 0.2375(2) 0.1284(3) 0.0168(5) Uani 1 1 d . . . . .
C4 C 0.8766(4) 0.8014(2) 0.9296(4) 0.0190(5) Uani 1 1 d . . . . .
C7 C 0.6091(4) 0.5417(3) 0.7768(4) 0.0209(5) Uani 1 1 d . . . . .
H7A H 0.675850 0.478026 0.769864 0.031 Uiso 1 1 calc R U . . .
H7B H 0.489929 0.540865 0.677501 0.031 Uiso 1 1 calc R U . . .
H7C H 0.599063 0.539841 0.887854 0.031 Uiso 1 1 calc R U . . .
C14 C 0.7862(4) 0.1355(3) 0.1307(4) 0.0216(5) Uani 1 1 d . . . . .
H14A H 0.699467 0.080321 0.060618 0.032 Uiso 1 1 calc R U . . .
H14B H 0.851593 0.109981 0.252532 0.032 Uiso 1 1 calc R U . . .
H14C H 0.869715 0.148616 0.080625 0.032 Uiso 1 1 calc R U . . .
C5 C 0.8740(4) 0.8408(2) 0.7744(4) 0.0178(5) Uani 1 1 d . . . . .
H5 H 0.930580 0.907911 0.776337 0.021 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
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
C1 Te C10 105.22(11) . . ?
C1 Te Cl2 91.43(7) . . ?
C10 Te Cl2 90.76(8) . . ?
C1 Te Cl1 89.33(7) . . ?
C10 Te Cl1 82.97(8) . . ?
Cl2 Te Cl1 173.66(3) . . ?
C13 O2 H2 109.5 . . ?
O1 C11 C12 123.5(2) . . ?
O1 C11 C10 116.8(2) . . ?
C12 C11 C10 119.7(2) . . ?
C13 C12 C11 119.8(2) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C2 C1 C6 121.7(2) . . ?
C2 C1 Te 124.9(2) . . ?
C6 C1 Te 113.37(18) . . ?
C3 C2 C1 117.1(3) . . ?
C3 C2 C7 118.1(2) . . ?
C1 C2 C7 124.8(2) . . ?
C4 C3 C2 122.6(3) . . ?
C4 C3 H3 118.7 . . ?
C2 C3 H3 118.7 . . ?
C5 C6 C1 118.4(2) . . ?
C5 C6 C9 118.1(3) . . ?
C1 C6 C9 123.5(2) . . ?
C11 C10 Te 104.28(18) . . ?
C11 C10 H10A 110.9 . . ?
Te C10 H10A 110.9 . . ?
C11 C10 H10B 110.9 . . ?
Te C10 H10B 110.9 . . ?
H10A C10 H10B 108.9 . . ?
C6 C9 H9A 109.5 . . ?
C6 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C6 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O2 C13 C12 120.7(3) . . ?
O2 C13 C14 114.7(2) . . ?
C12 C13 C14 124.6(3) . . ?
C3 C4 C5 118.5(3) . . ?
C3 C4 C8 120.8(3) . . ?
C5 C4 C8 120.6(3) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C4 C5 C6 121.6(3) . . ?
C4 C5 H5 119.2 . . ?
C6 C5 H5 119.2 . . ?
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
Te C1 2.126(3) . ?
Te C10 2.141(3) . ?
Te Cl2 2.4793(16) . ?
Te Cl1 2.5337(17) . ?
O2 C13 1.321(3) . ?
O2 H2 0.8400 . ?
O1 C11 1.262(3) . ?
C11 C12 1.408(4) . ?
C11 C10 1.512(4) . ?
C12 C13 1.378(4) . ?
C12 H12 0.9500 . ?
C1 C2 1.406(4) . ?
C1 C6 1.406(4) . ?
C2 C3 1.399(4) . ?
C2 C7 1.502(4) . ?
C3 C4 1.387(4) . ?
C3 H3 0.9500 . ?
C6 C5 1.391(4) . ?
C6 C9 1.511(4) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C8 C4 1.507(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C13 C14 1.477(4) . ?
C4 C5 1.391(4) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C5 H5 0.9500 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H2 O1 0.84 1.74 2.498(3) 148.4 . yes
C12 H12 Cl2 0.95 2.91 3.704(3) 141.8 2_646 yes
C14 H14A O1 0.98 2.52 3.501(4) 176.4 2_645 yes
C14 H14B Cl1 0.98 2.84 3.803(4) 166.8 2_746 yes
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 C11 C12 C13 1.6(4) . . . . ?
C10 C11 C12 C13 -179.8(3) . . . . ?
C6 C1 C2 C3 -3.3(4) . . . . ?
Te C1 C2 C3 178.9(2) . . . . ?
C6 C1 C2 C7 175.1(3) . . . . ?
Te C1 C2 C7 -2.8(4) . . . . ?
C1 C2 C3 C4 1.7(4) . . . . ?
C7 C2 C3 C4 -176.8(3) . . . . ?
C2 C1 C6 C5 2.9(4) . . . . ?
Te C1 C6 C5 -179.0(2) . . . . ?
C2 C1 C6 C9 -176.2(3) . . . . ?
Te C1 C6 C9 1.9(3) . . . . ?
O1 C11 C10 Te -35.1(3) . . . . ?
C12 C11 C10 Te 146.2(2) . . . . ?
C11 C12 C13 O2 -0.4(4) . . . . ?
C11 C12 C13 C14 179.9(3) . . . . ?
C2 C3 C4 C5 0.2(5) . . . . ?
C2 C3 C4 C8 179.8(3) . . . . ?
C3 C4 C5 C6 -0.6(4) . . . . ?
C8 C4 C5 C6 179.8(3) . . . . ?
C1 C6 C5 C4 -0.9(4) . . . . ?
C9 C6 C5 C4 178.2(3) . . . . ?
