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_7714398
_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
'C28 H29 O5 Te2, C28 H28 O5 Te2, 4(B F4), 5(C3 H3)'
_chemical_formula_sum            'C71 H72 B4 F16 O10 Te4'
_chemical_formula_weight         1942.92
_chemical_name_systematic        Macrocycle
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-03-19
_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                90
_cell_angle_beta                 97.0650(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.0516(2)
_cell_length_b                   17.0082(3)
_cell_length_c                   26.0697(4)
_cell_measurement_reflns_used    29640
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      26.8040
_cell_measurement_theta_min      2.0850
_cell_volume                     7503.3(2)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_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      100.0(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_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    -13.00  21.00   0.50   15.32    --  -14.97 -94.00  30.00   68
  2  \w     10.00  71.00   0.50   15.32    --   16.22-125.00  60.00  122
  3  \w    -33.00  43.00   0.50   15.32    --   16.22 -94.00 120.00  152
  4  \w    -13.00  12.00   0.50   15.32    --  -14.97 -89.00 169.00   50
  5  \w    -44.00  40.00   0.50   15.32    --   16.22 -89.00 169.00  168
  6  \w    -54.00  -7.00   0.50   15.32    --   16.22 -77.00 150.00   94
  7  \w    -81.00 -10.00   0.50   15.32    --  -14.97 -77.00 120.00  142
  8  \w     -1.00  39.00   0.50   15.32    --   16.22  45.00 120.00   80
  9  \w    -69.00 -14.00   0.50   15.32    --  -14.97 125.00   0.00  110
 10  \w    -46.00 -12.00   0.50   15.32    --  -14.97 125.00 -60.00   68
 11  \w     -8.00  25.00   0.50   15.32    --  -14.97  89.00 -74.00   66
 12  \w    -43.00 -15.00   0.50   15.32    --  -14.97  89.00 -74.00   56
 13  \w    -17.00  29.00   0.50   15.32    --   16.22  89.00 -74.00   92
 14  \w    -12.00  81.00   0.50   15.32    --   16.22  77.00 -90.00  186
 15  \w    -38.00 -13.00   0.50   15.32    --  -14.97 125.00 -90.00   50
 16  \w    -68.00 -33.00   0.50   15.32    --  -14.97 125.00 120.00   70
;
_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      0.0245143000
_diffrn_orient_matrix_UB_12      0.0256881000
_diffrn_orient_matrix_UB_13      0.0163356000
_diffrn_orient_matrix_UB_21      -0.0008744000
_diffrn_orient_matrix_UB_22      0.0275895000
_diffrn_orient_matrix_UB_23      -0.0204475000
_diffrn_orient_matrix_UB_31      -0.0340102000
_diffrn_orient_matrix_UB_32      0.0178347000
_diffrn_orient_matrix_UB_33      0.0081322000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0817
_diffrn_reflns_av_unetI/netI     0.0607
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            67629
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.860
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.635
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.61525
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
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    1.720
_exptl_crystal_description       block
_exptl_crystal_F_000             3800
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         3.357
_refine_diff_density_min         -1.449
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     954
_refine_ls_number_reflns         13201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0594
_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^)+(0.0793P)^2^+35.8211P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1427
_refine_ls_wR_factor_ref         0.1499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10861
_reflns_number_total             13201
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02746e2.cif
_cod_data_source_block           vb62
_cod_original_cell_volume        7503.2(2)
_cod_database_code               7714398
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C71H71F16O10B4Te4
_shelx_estimated_absorpt_t_max   0.780
_shelx_estimated_absorpt_t_min   0.623
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C013(H01A,H01B)
2.b Aromatic/amide H refined with riding coordinates:
 C011(H011), C012(H012), C015(H015), C016(H016), C017(H017), C019(H019),
 C01A(H01E), C01B(H01C), C01C(H01D), C01D(H01H), C01F(H01F), C01G(H01G),
 C01J(H01J), C01K(H01K), C01L(H01L), C01M(H01M), C01N(H01N), C01O(H01O),
 C01P(H01P), C01Q(H01Q), C01R(H01R), C01S(H01S), C01T(H01T), C01U(H01U),
 C01V(H01V), C01X(H01X), C01Y(H01Y), C01Z(H01Z), C021(H021), C025(H025),
 C026(H026), C027(H027), C029(H029), C02H(H02Y), C02I(H9AA), C02J(H3AA),
 C02K(H4AA), C02L(H5AA), C02M(H02Z), C02N(H02), C02O(H0AA), C02R(H6AA),
 C02S(H7AA), C02U(H8AA), C02V(H1AA), C02W(H2AA)
2.c Idealised Me refined as rotating group:
 C020(H02A,H02B,H02C), C028(H02M,H02N,H02O), C02B(H02P,H02Q,H02R), C02C(H02D,
 H02E,H02F), C02E(H02G,H02H,H02I), C02G(H02J,H02K,H02L), C02T(H02S,H02T,H02U),
 C02X(H02V,H02W,H02X)
;
_shelx_res_checksum              94858
_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 1.680
_oxdiff_exptl_absorpt_empirical_full_min 0.408