Electrocatalytic Hydrogen Evolution Mediated by an Organotelluroxane Macrocycle Stabilized through Secondary Interactions
Narsimhulu, Gujju; Samuel, Calvin; Sathish, Palani; Dasari, Sai Hemanth Kumar; Krishnamoorthy, Kothandam; Viswanathan, Baskar; Dalton Transactions  (2023) –; doi:10.1039/D3DT02746E

data_7714399
_publ_section_title
;
 Electrocatalytic Hydrogen Evolution Mediated by an Organotelluroxane
 Macrocycle Stabilized through Secondary Interactions
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02746E
_journal_year                    2023
_chemical_formula_moiety         'C21 H21 O3 Te, B F4'
_chemical_formula_sum            'C21 H21 B F4 O3 Te'
_chemical_formula_weight         535.79
_chemical_name_systematic
'tris(p-methoxyphenyl)Telluronium tetraflouroborate'
_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             2022-03-16
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2018.12.18 svn.r3554 for Rigaku Oxford Diffraction, GUI svn.r1)
;
_audit_update_record
;
2022-03-21 deposited with the CCDC.	2023-11-06 downloaded from the CCDC.
;
_cell_angle_alpha                110.245(2)
_cell_angle_beta                 97.9550(10)
_cell_angle_gamma                104.2830(10)
_cell_formula_units_Z            2
_cell_length_a                   10.2455(2)
_cell_length_b                   10.5162(2)
_cell_length_c                   10.9829(2)
_cell_measurement_reflns_used    12494
_cell_measurement_temperature    106(9)
_cell_measurement_theta_max      26.8880
_cell_measurement_theta_min      2.0430
_cell_volume                     1042.82(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      106(9)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.954
_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    -46.00 -20.00   0.50    3.00    --   16.22 -67.00  57.00   52
  2  \w    -10.00  42.00   0.50    3.00    --   16.22 -67.00  57.00  104
  3  \w     50.00  75.00   0.50    3.00    --   16.22 -15.00  60.00   50
  4  \w      0.00  55.00   0.50    3.00    --  -14.97  45.00  60.00  110
  5  \w    -37.00  21.00   0.50    3.00    --  -14.97 -94.00 150.00  116
  6  \w    -63.00  -6.00   0.50    3.00    --  -14.97 -67.00  57.00  114
  7  \w    -37.00  21.00   0.50    3.00    --  -14.97 -94.00  30.00  116
  8  \w    -36.00  17.00   0.50    3.00    --   16.22 -94.00  30.00  106
  9  \w    -63.00  28.00   0.50    3.00    --   16.22 -15.00  60.00  182
 10  \w    -65.00 -18.00   0.50    3.00    --  -14.97 125.00 -30.00   94
 11  \w    -43.00 -17.00   0.50    3.00    --  -14.97 125.00 -60.00   52
 12  \w    -44.00  55.00   0.50    3.00    --  -14.97  67.00-168.00  198
 13  \w    -31.00  20.00   0.50    3.00    --  -14.97 -94.00 -90.00  102
 14  \w     32.00  58.00   0.50    3.00    --   16.22-125.00 -90.00   52
 15  \w     -6.00  44.00   0.50    3.00    --   16.22 -94.00-120.00  100
 16  \w    -41.00  59.00   0.50    3.00    --  -14.97  30.00-180.00  200
 17  \w     45.00  85.00   0.50    3.00    --   16.22  67.00-168.00   80
 18  \w     20.00  51.00   0.50    3.00    --   16.22  45.00-180.00   62
 19  \w    -56.00  32.00   0.50    3.00    --   16.22 -30.00 -90.00  176
 20  \w    -85.00  -6.00   0.50    3.00    --  -14.97 -45.00-120.00  158
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0531131000
_diffrn_orient_matrix_UB_12      -0.0176722000
_diffrn_orient_matrix_UB_13      -0.0308879000
_diffrn_orient_matrix_UB_21      0.0161002000
_diffrn_orient_matrix_UB_22      -0.0318839000
_diffrn_orient_matrix_UB_23      0.0449844000
_diffrn_orient_matrix_UB_31      -0.0485007000
_diffrn_orient_matrix_UB_32      -0.0664586000
_diffrn_orient_matrix_UB_33      -0.0454542000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15561
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.962
_diffrn_reflns_theta_min         2.039
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.482
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74448
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       plate
_exptl_crystal_F_000             528
_exptl_crystal_recrystallization_method 'Direct evopuration'
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.303
_refine_diff_density_min         -0.726
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         4326
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0294
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0229P)^2^+1.0127P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0595
_refine_ls_wR_factor_ref         0.0610
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4023
_reflns_number_total             4326
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02746e2.cif
_cod_data_source_block           vb115a
_cod_database_code               7714399
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.866
_shelx_estimated_absorpt_t_min   0.384
_reflns_odcompleteness_completeness 99.23
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C6(H6), C9(H9), C19(H19), C20(H20), C5(H5), C17(H17), C13(H13),
 C16(H16), C3(H3), C2(H2), C12(H12)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C21(H21A,H21B,H21C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              67990
_olex2_exptl_crystal_mounting_method 'Mounted on glass fiber tip '
_olex2_submission_original_sample_id Gnrg-Vb194
_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 1.947
_oxdiff_exptl_absorpt_empirical_full_min 0.658