Exploring the reactivity of L-tellurocystine, Te-protected tellurocysteine conjugates and diorganodiselenides towards hydrogen peroxide: synthesis and molecular structure analysis
Tripathi, Abhishek; Deka, Rajesh; Butcher, Ray J.; Turner, David R.; Deacon, Glen B.; Singh, Harkesh B.; New Journal of Chemistry 46 (2022) 10550–10559; doi:10.1039/D2NJ00997H

data_7061577
_publ_section_title
;
 Exploring the reactivity of L-tellurocystine, Te-protected
 tellurocysteine conjugates and diorganodiselenides towards hydrogen
 peroxide: synthesis and molecular structure analysis
;
_journal_issue                   22
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              10550
_journal_page_last               10559
_journal_paper_doi               10.1039/D2NJ00997H
_journal_volume                  46
_journal_year                    2022
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C3 H6 Br3 N O2 Te, 2(H2 O)'
_chemical_formula_sum            'C3 H10 Br3 N O4 Te'
_chemical_formula_weight         491.45
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-02
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-09-28 deposited with the CCDC.	2022-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.85996(15)
_cell_length_b                   9.5789(3)
_cell_length_c                   20.0889(5)
_cell_measurement_reflns_used    7451
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      32.1010
_cell_measurement_theta_min      3.6120
_cell_volume                     1127.63(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.850
_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     -5.00  38.00   0.50    1.00    --    7.87  53.00  74.00   86
  2  \w    -25.00  56.00   0.50    1.00    --   -8.65  67.00-104.00  162
  3  \w    -17.00  24.00   0.50    1.00    --   -8.65 -99.00 -90.00   82
  4  \w    -72.00   0.00   0.50    1.00    --   -8.65 -57.00 150.00  144
  5  \w    -21.00  21.00   0.50    1.00    --   -8.65 -99.00  60.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0775417000
_diffrn_orient_matrix_UB_12      0.0082720000
_diffrn_orient_matrix_UB_13      0.0268276000
_diffrn_orient_matrix_UB_21      -0.0033150000
_diffrn_orient_matrix_UB_22      -0.0734655000
_diffrn_orient_matrix_UB_23      0.0043316000
_diffrn_orient_matrix_UB_31      0.0929101000
_diffrn_orient_matrix_UB_32      0.0042880000
_diffrn_orient_matrix_UB_33      0.0225295000
_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  0.0359
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.850
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            10892
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.852
_diffrn_reflns_theta_min         3.622
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    13.249
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51398
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.895
_exptl_crystal_description       block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.952
_refine_diff_density_min         -1.038
_refine_diff_density_rms         0.146
_refine_ls_abs_structure_details
;
 Flack x determined using 1158 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.016(6)
_refine_ls_extinction_coef       0.0022(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     123
_refine_ls_number_reflns         3186
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0245
_refine_ls_R_factor_gt           0.0222
_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^)+(0.0174P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0429
_refine_ls_wR_factor_ref         0.0433
_reflns_Friedel_coverage         0.672
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.785
_reflns_number_gt                3014
_reflns_number_total             3186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj00997h2.cif
_cod_data_source_block           at-te-3br
_cod_original_cell_volume        1127.62(5)
_cod_database_code               7061577
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         CHNOTeBr
_shelx_estimated_absorpt_t_max   0.351
_shelx_estimated_absorpt_t_min   0.177
_reflns_odcompleteness_completeness 99.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O3-H3A = O3-H3B
 0.85 with sigma of 0.02
 O4-H4A = O4-H4B
 0.85 with sigma of 0.02
 H3A-H3B
 1.34 with sigma of 0.04
 H4A-H4B
 1.34 with sigma of 0.04
3.a Ternary CH refined with riding coordinates:
 C2(H2)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1D,H1E)
3.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
;
_shelx_res_checksum              79606
_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 1.821
_oxdiff_exptl_absorpt_empirical_full_min 0.744