Tellurolate: an effective Te-atom transfer reagent to prepare the triad of group 5 metal bis(tellurides).
Senthil, Shuruthi; Kwon, Seongyeon; Kong, Richard Y.; MacMillan, Samantha N.; Zatsepin, Pavel; Gau, Michael R.; Carroll, Patrick J.; Baik, Mu-Hyun; Lancaster, Kyle M.; Mindiola, Daniel J.; Chemical science 14 (2023) 12277–12282; doi:10.1039/d3sc03470d

data_1570059
_publ_section_title
;
 Tellurolate: an effective Te-atom transfer reagent to prepare the triad
 of group 5 metal bis(tellurides).
;
_journal_issue                   43
_journal_name_full               'Chemical science'
_journal_page_first              12277
_journal_page_last               12282
_journal_paper_doi               10.1039/d3sc03470d
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C4 H11 Si Te, C16 H32 Li O8'
_chemical_formula_sum            'C20 H43 Li O8 Si Te'
_chemical_formula_weight         574.17
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-04-11
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6396)
;
_audit_update_record
;
2023-05-10 deposited with the CCDC.	2023-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9891(2)
_cell_length_b                   19.9870(3)
_cell_length_c                   12.3245(2)
_cell_measurement_reflns_used    43212
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.4710
_cell_measurement_theta_min      1.9340
_cell_volume                     2706.94(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.122a (Rigaku OD, 2021)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'HPC area detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix 3000HE'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -59.00   9.00   0.50   14.00    --  -14.00 -57.00  90.00  136
  2  \w    -41.00  60.00   0.50   14.00    --  -14.00  19.00 -90.00  202
  3  \w    -22.00  15.00   0.50   14.00    --  -14.00 -80.00-177.31   74
  4  \w    -59.00   9.00   0.50   14.00    --  -14.00 -57.00 -90.00  136
  5  \w    -42.00  25.00   0.50   14.00    --  -14.00  77.00 -30.00  134
  6  \w    -25.00  14.00   0.50   14.00    --  -14.00 -77.00 -90.00   78
  7  \w    -22.00  15.00   0.50   14.00    --  -14.00 -80.00 130.03   74
  8  \w    -25.00  14.00   0.50   14.00    --  -14.00 -77.00-120.00   78
  9  \w    -22.00  15.00   0.50   14.00    --  -14.00 -80.00 150.40   74
 10  \w    -24.00  15.00   0.50   14.00    --  -14.00 -78.00  38.87   78
 11  \w    -22.00  15.00   0.50   14.00    --  -14.00 -80.00-133.48   74
 12  \w    -25.00  14.00   0.50   14.00    --  -14.00 -77.00  90.00   78
 13  \w    -25.00  14.00   0.50   14.00    --  -14.00 -77.00 -30.00   78
 14  \w    -22.00  15.00   0.50   14.00    --  -14.00 -80.00  43.47   74
 15  \w    -25.00  43.00   0.50   14.00    --   14.62 -77.00-105.92  136
 16  \w     -2.00  83.00   0.50   14.00    --   14.62  37.00 150.00  170
 17  \w    -59.00   5.00   0.50   14.00    --   14.62 -19.00 -90.00  128
 18  \w    -22.00  44.00   0.50   14.00    --   14.62 -80.00  43.95  132
 19  \w    -53.00  21.00   0.50   14.00    --   14.62 -37.00   0.00  148
 20  \w    -53.00  37.00   0.50   14.00    --   14.62 -57.00-180.00  180
 21  \w    -53.00  21.00   0.50   14.00    --   14.62 -37.00-150.00  148
 22  \w    -53.00  21.00   0.50   14.00    --   14.62 -37.00 -30.00  148
 23  \w     -8.00  59.00   0.50   14.00    --   14.62  57.00-120.00  134
 24  \w    -12.00  89.00   0.50   14.00    --   14.62  19.00  90.00  202
 25  \w    -59.00   5.00   0.50   14.00    --   14.62 -19.00  90.00  128
 26  \w    -13.00  25.00   0.50   14.00    --   14.62  77.00  90.00   76
 27  \w    -59.00   5.00   0.50   14.00    --   14.62 -19.00-120.00  128
 28  \w    -22.00  44.00   0.50   14.00    --   14.62 -80.00 139.98  132
 29  \w    -59.00   0.00   0.50   14.00    --   14.62 -19.00  30.00  118
 30  \w    -14.00  37.00   0.50   14.00    --   14.62 -80.00  75.13  102
 31  \w    -58.00 -24.00   0.50   14.00    --   14.62 -19.00 -30.00   68
 32  \w     -4.00  25.00   0.50   14.00    --   14.62  77.00  30.00   58
 33  \w    -58.00  -3.00   0.50   14.00    --   14.62 -19.00 150.00  110
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-i'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0213218000
_diffrn_orient_matrix_UB_12      -0.0542597000
_diffrn_orient_matrix_UB_13      0.0015301000
_diffrn_orient_matrix_UB_21      -0.0602247000
_diffrn_orient_matrix_UB_22      0.0183954000
_diffrn_orient_matrix_UB_23      -0.0059056000
_diffrn_orient_matrix_UB_31      0.0092280000
_diffrn_orient_matrix_UB_32      -0.0054863000
_diffrn_orient_matrix_UB_33      -0.0349546000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            79546
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.476
_diffrn_reflns_theta_min         1.941
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.181
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66347
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.409
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3200
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0242
_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^)+(0.0200P)^2^+1.7940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0536
_reflns_number_gt                2796
_reflns_number_total             3200
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03470d2.cif
_cod_data_source_block           9871_complex1
_cod_depositor_comments
'Adding full bibliography for 1570059--1570061.cif.'
_cod_database_code               1570059
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              76693
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.476
_oxdiff_exptl_absorpt_empirical_full_min 0.776