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_1570061
_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         'C26 H40 N P2 Ta Te2, 2.5(C4 H8 O)'
_chemical_formula_sum            'C36 H60 N O2.5 P2 Ta Te2'
_chemical_formula_weight         1044.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-05-08
_audit_creation_method
;
Olex2 1.5
(compiled 2021.10.07 svn.r9718050b for OlexSys, GUI svn.r6410)
;
_audit_update_record
;
2023-05-10 deposited with the CCDC.	2023-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                64.384(2)
_cell_angle_beta                 77.963(2)
_cell_angle_gamma                88.962(2)
_cell_formula_units_Z            2
_cell_length_a                   11.5337(2)
_cell_length_b                   13.6583(3)
_cell_length_c                   14.3715(3)
_cell_measurement_reflns_used    36743
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5230
_cell_measurement_theta_min      2.1230
_cell_volume                     1989.87(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.104a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (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-6000HE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_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    -13.00  84.00   0.50   19.00    --   14.70  77.00  27.00  194
  2  \w    -55.00  43.00   0.50   19.00    --   14.70 -77.00 -97.00  196
  3  \w    -22.00  15.00   0.50   19.00    --  -14.00 -80.00  49.49   74
  4  \w    -25.00  14.00   0.50   19.00    --  -14.00 -77.00 150.00   78
  5  \w    -31.00  54.00   0.50   19.00    --  -14.00  37.00   0.00  170
  6  \w    -22.00  15.00   0.50   19.00    --  -14.00 -80.00-112.74   74
  7  \w    -82.00   3.00   0.50   19.00    --  -14.00 -37.00  60.00  170
  8  \w    -22.00  15.00   0.50   19.00    --  -14.00 -80.00-128.27   74
  9  \w    -42.00  56.00   0.50   19.00    --  -14.00  77.00  27.00  196
 10  \w    -37.00  54.00   0.50   19.00    --  -14.00  57.00 -60.00  182
 11  \w    -22.00  15.00   0.50   19.00    --  -14.00 -80.00  34.81   74
 12  \w    -22.00  15.00   0.50   19.00    --  -14.00 -80.00 -21.06   74
 13  \w    -23.00  15.00   0.50   19.00    --  -14.00 -79.00 -74.64   76
 14  \w    -12.00  53.00   0.50   19.00    --  -14.00  37.00-120.00  130
 15  \w    -20.00   7.00   0.50   19.00    --  -14.00 -80.00-170.65   54
 16  \w    -76.00 -49.00   0.50   19.00    --  -14.00 -77.00 -97.00   54
 17  \w    -24.00   1.00   0.50   19.00    --  -14.00 -78.00 141.04   50
 18  \w    -54.00   4.00   0.50   19.00    --   14.70 -19.00 -90.00  116
 19  \w    -58.00  -3.00   0.50   19.00    --   14.70 -19.00 150.00  110
 20  \w     -7.00  19.00   0.50   19.00    --   14.70  80.00-139.87   52
 21  \w    -32.00  37.00   0.50   19.00    --   14.70 -57.00-180.00  138
 22  \w    -59.00   5.00   0.50   19.00    --   14.70 -19.00  90.00  128
 23  \w     -9.00  21.00   0.50   19.00    --   14.70  77.00-180.00   60
 24  \w    -43.00 -16.00   0.50   19.00    --   14.70 -19.00 -60.00   54
 25  \w     -8.00  58.00   0.50   19.00    --   14.70  57.00 -30.00  132
 26  \w    -11.00  20.00   0.50   19.00    --   14.70  79.00  49.58   62
 27  \w    -52.00   6.00   0.50   19.00    --   14.70 -37.00  30.00  116
 28  \w    -12.00  14.00   0.50   19.00    --   14.70  77.00-150.00   52
 29  \w    -58.00  -1.00   0.50   19.00    --   14.70 -19.00  60.00  114
 30  \w    -24.00  26.00   0.50   19.00    --   14.70 -77.00-180.00  100
 31  \w    -14.00  14.00   0.50   19.00    --   14.70  80.00 141.59   56
 32  \w    -55.00   4.00   0.50   19.00    --   14.70 -19.00 -30.00  118
 33  \w     -8.00  58.00   0.50   19.00    --   14.70  57.00 150.00  132
 34  \w     -7.00  58.00   0.50   19.00    --   14.70  57.00-120.00  130
 35  \w     -8.00  20.00   0.50   19.00    --   14.70  79.00 -60.38   56
 36  \w      9.00  36.00   0.50   19.00    --   14.70 -75.00  66.96   54
 37  \w    -20.00  43.00   0.50   19.00    --   14.70 -80.00   2.15  126
 38  \w    -42.00   5.00   0.50   19.00    --   14.70 -19.00 120.00   94
;
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0526274000
_diffrn_orient_matrix_UB_12      -0.0268164000
_diffrn_orient_matrix_UB_13      0.0387101000
_diffrn_orient_matrix_UB_21      -0.0326981000
_diffrn_orient_matrix_UB_22      0.0437351000
_diffrn_orient_matrix_UB_23      -0.0271725000
_diffrn_orient_matrix_UB_31      -0.0119049000
_diffrn_orient_matrix_UB_32      -0.0265953000
_diffrn_orient_matrix_UB_33      -0.0302534000
_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  0.0489
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            60965
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         1.811
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.311
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53299
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.744
_exptl_crystal_description       plate
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
_refine_diff_density_max         3.419
_refine_diff_density_min         -2.576
_refine_diff_density_rms         0.216
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         9059
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0575
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0817P)^2^+11.0964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1396
_reflns_number_gt                7742
_reflns_number_total             9059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03470d2.cif
_cod_data_source_block           9833_complex3
_cod_depositor_comments
'Adding full bibliography for 1570059--1570061.cif.'
_cod_original_cell_volume        1989.88(8)
_cod_original_formula_sum        'C36 H60 N O2.50 P2 Ta Te2'
_cod_database_code               1570061
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              82752
_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 1.456
_oxdiff_exptl_absorpt_empirical_full_min 0.621