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_1570060
_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 Nb P2 Te2, 2.5(C4 H8 O)'
_chemical_formula_sum            'C36 H60 N Nb O2.5 P2 Te2'
_chemical_formula_weight         956.90
_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                64.365(2)
_cell_angle_beta                 77.8010(10)
_cell_angle_gamma                88.8530(10)
_cell_formula_units_Z            2
_cell_length_a                   11.5657(2)
_cell_length_b                   13.6873(2)
_cell_length_c                   14.3677(2)
_cell_measurement_reflns_used    37264
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.4580
_cell_measurement_theta_min      2.1210
_cell_volume                     1997.68(6)
_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 3000HE'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_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    -47.00  93.00   0.50   20.86    --   14.70   9.00 -86.00  280
  2  \w    -63.00   4.00   0.50   20.86    --   14.70  -9.00  98.00  134
  3  \w    -47.00  93.00   0.50   20.86    --   14.70   9.00 -86.00  280
  4  \w    -82.00   3.00   0.50   20.86    --  -14.00 -37.00 -30.00  170
  5  \w    -47.00  64.00   0.50   20.86    --  -14.00   9.00 -86.00  222
  6  \w    -22.00  15.00   0.50   20.86    --  -14.00 -80.00 135.27   74
  7  \w    -43.00  22.00   0.50   20.86    --  -14.00  80.00-110.74  130
  8  \w    -25.00  14.00   0.50   20.86    --  -14.00 -77.00 -16.82   78
  9  \w    -22.00  15.00   0.50   20.86    --  -14.00 -80.00 161.99   74
 10  \w    -24.00  15.00   0.50   20.86    --  -14.00 -78.00 -65.07   78
 11  \w    -48.00   1.00   0.50   20.86    --  -14.00 -57.00 -30.00   98
 12  \w    -88.00 -30.00   0.50   20.86    --  -14.00  -9.00  98.00  116
 13  \w    -14.00  13.00   0.50   20.86    --  -14.00 -80.00 -18.95   54
 14  \w    -30.00   6.00   0.50   20.86    --  -14.00  37.00   0.00   72
 15  \w    -36.00  10.00   0.50   20.86    --  -14.00  77.00 -30.00   92
 16  \w    -22.00   3.00   0.50   20.86    --  -14.00 -80.00-106.38   50
 17  \w    -20.00   7.00   0.50   20.86    --  -14.00 -80.00 -94.37   54
 18  \w    -59.00  -4.00   0.50   20.86    --  -14.00 -57.00  60.00  110
 19  \w    -58.00  -1.00   0.50   20.86    --  -14.00 -57.00 150.00  114
 20  \w    -28.00  -1.00   0.50   20.86    --  -14.00  77.00   0.00   54
 21  \w    -15.00  15.00   0.50   20.86    --  -14.00 -80.00  94.60   60
 22  \w    -24.00  14.00   0.50   20.86    --  -14.00 -77.00  60.00   76
 23  \w    -17.00  12.00   0.50   20.86    --  -14.00 -80.00  16.51   58
 24  \w    -21.00  44.00   0.50   20.86    --   14.70 -80.00 174.17  130
 25  \w     -7.00  43.00   0.50   20.86    --   14.70  57.00 -30.00  100
 26  \w    -14.00  11.00   0.50   20.86    --   14.70  80.00 -31.30   50
 27  \w     39.00  82.00   0.50   20.86    --   14.70  37.00 -60.00   86
 28  \w     -1.00  41.00   0.50   20.86    --   14.70  57.00-180.00   84
 29  \w      5.00  32.00   0.50   20.86    --   14.70  37.00 -60.00   54
 30  \w    -12.00  16.00   0.50   20.86    --   14.70  78.00 140.54   56
 31  \w    -59.00  -5.00   0.50   20.86    --   14.70 -19.00 -90.00  108
 32  \w     -2.00  53.00   0.50   20.86    --   14.70  57.00 120.00  110
 33  \w     -8.00  58.00   0.50   20.86    --   14.70  57.00-120.00  132
 34  \w    -12.00  18.00   0.50   20.86    --   14.70  77.00 -60.00   60
 35  \w    -18.00   8.00   0.50   20.86    --   14.70 -80.00 118.07   52
 36  \w    -58.00   4.00   0.50   20.86    --   14.70 -19.00   0.00  124
 37  \w     34.00  85.00   0.50   20.86    --   14.70  19.00 120.00  102
 38  \w     -8.00  17.00   0.50   20.86    --   14.70  80.00  15.87   50
 39  \w     -6.00  24.00   0.50   20.86    --   14.70  77.00 -30.00   60
 40  \w     23.00  59.00   0.50   20.86    --   14.70  57.00  60.00   72
;
_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      0.0552233000
_diffrn_orient_matrix_UB_12      0.0265870000
_diffrn_orient_matrix_UB_13      -0.0066171000
_diffrn_orient_matrix_UB_21      0.0293144000
_diffrn_orient_matrix_UB_22      -0.0457824000
_diffrn_orient_matrix_UB_23      -0.0006797000
_diffrn_orient_matrix_UB_31      0.0073474000
_diffrn_orient_matrix_UB_32      0.0228655000
_diffrn_orient_matrix_UB_33      -0.0558012000
_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  0.0470
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_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            62949
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         2.135
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.844
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.591
_exptl_crystal_description       plank
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.631
_refine_diff_density_min         -1.177
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         9088
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0743P)^2^+8.1562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1464
_reflns_number_gt                7517
_reflns_number_total             9088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc03470d2.cif
_cod_data_source_block           9832_complex2
_cod_depositor_comments
'Adding full bibliography for 1570059--1570061.cif.'
_cod_original_formula_sum        'C36 H60 N Nb O2.50 P2 Te2'
_cod_database_code               1570060
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              57261
_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 1.909
_oxdiff_exptl_absorpt_empirical_full_min 0.582