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_7714401
_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         '2(C28 H28 O5 Te2), 4(Cl O4), 5(C3 H3)'
_chemical_formula_sum            'C71 H71 Cl4 O26 Te4'
_chemical_formula_weight         1992.47
_chemical_name_systematic        'perchlorate 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     iterative
_audit_creation_date             2021-04-12
_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                 97.4190(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.14200(10)
_cell_length_b                   17.20420(10)
_cell_length_c                   26.0805(2)
_cell_measurement_reflns_used    60868
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      26.9820
_cell_measurement_theta_min      2.0930
_cell_volume                     7627.12(9)
_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    'olex2.solve (Bourhis et al., 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 0.999
_diffrn_measured_fraction_theta_max 0.961
_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    -51.00 -17.00   0.50   10.00    --   16.22 -44.00 -52.00   68
  2  \w    -44.00  -1.00   0.50   10.00    --  -14.97 -44.00 -52.00   86
  3  \w    -36.00  22.00   0.50   10.00    --  -14.97 -94.00 -60.00  116
  4  \w     42.00  68.00   0.50   10.00    --   16.22-125.00 -90.00   52
  5  \w      2.00  35.00   0.50   10.00    --   16.22 -30.00-150.00   66
  6  \w    -17.00   9.00   0.50   10.00    --  -14.97 -61.00 -90.00   52
  7  \w    -31.00  18.00   0.50   10.00    --  -14.97 -94.00-120.00   98
  8  \w     10.00  35.00   0.50   10.00    --   16.22-125.00 -90.00   50
  9  \w    -56.00  39.00   0.50   10.00    --   16.22 -30.00 -30.00  190
 10  \w    -69.00 -43.00   0.50   10.00    --  -14.97 -61.00 -90.00   52
 11  \w    -82.00 -57.00   0.50   10.00    --  -14.97 -44.00 -52.00   50
 12  \w    -54.00 -20.00   0.50   10.00    --   16.22 -30.00-150.00   68
 13  \w    -36.00 -11.00   0.50   10.00    --  -14.97 125.00 -60.00   50
 14  \w    -40.00 -10.00   0.50   10.00    --  -14.97 125.00   0.00   60
 15  \w    -66.00 -23.00   0.50   10.00    --  -14.97 125.00  60.00   86
 16  \w    -66.00 -11.00   0.50   10.00    --  -14.97 125.00  90.00  110
 17  \w    -36.00  54.00   0.50   10.00    --  -14.97  45.00 120.00  180
 18  \w     47.00  72.00   0.50   10.00    --   16.22  44.00  98.00   50
 19  \w     23.00  51.00   0.50   10.00    --  -14.97  44.00  98.00   56
 20  \w    -69.00 -43.00   0.50   10.00    --  -14.97 125.00 -30.00   52
 21  \w      7.00  32.00   0.50   10.00    --   16.22  44.00  98.00   50
;
_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      -0.0333393000
_diffrn_orient_matrix_UB_12      0.0208888000
_diffrn_orient_matrix_UB_13      0.0059943000
_diffrn_orient_matrix_UB_21      -0.0104013000
_diffrn_orient_matrix_UB_22      0.0086773000
_diffrn_orient_matrix_UB_23      -0.0265891000
_diffrn_orient_matrix_UB_31      -0.0228147000
_diffrn_orient_matrix_UB_32      -0.0344704000
_diffrn_orient_matrix_UB_33      -0.0030989000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0230
_diffrn_reflns_av_unetI/netI     0.0182
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            80531
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.937
_diffrn_reflns_theta_min         1.970
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.734
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66136
_exptl_absorpt_correction_type   empirical
_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 brownish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_description       cube
_exptl_crystal_F_000             3924
_exptl_crystal_preparation
'silver perchlorate, organotellurium refluxion in benzene for 3 hours'
_exptl_crystal_recrystallization_method 'direct evopuration in a 5 ml voil'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.285
_refine_diff_density_min         -1.022
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     954
_refine_ls_number_reflns         15871
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0266
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0126P)^2^+13.1810P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0521
_refine_ls_wR_factor_ref         0.0528
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15185
_reflns_number_total             15871
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02746e2.cif
_cod_data_source_block           vb119
_cod_original_cell_volume        7627.13(9)
_cod_database_code               7714401
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C56 H56 Te4 Cl4 O26'
_reflns_odcompleteness_completeness 99.44
_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:
 C20(H20), C37(H37), C27(H27), C19(H19), C17(H17), C3(H3), C41(H41), C51(H51),
 C55(H55), C54(H54), C16(H16), C30(H30), C2(H2), C5(H5), C6(H6), C38(H38),
 C47(H47), C40(H40), C13(H13), C33(H33), C34(H34), C9(H9), C48(H48), C24(H24),
 C31(H31), C26(H26), C45(H45), C23(H23), C44(H44), C10(H10), C12(H12), C52(H52),
  C02A(H02A), C02E(H02E), C02F(H02F), C02G(H02G), C02H(H02H), C02I(H02I),
 C02L(H02L), C02M(H02M), C02N(H02N), C02P(H02P), C02Q(H02Q), C02R(H02R),
 C02T(H02T), C02U(H02U), C02X(H02X)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C56(H56A,H56B,H56C), C28(H28A,H28B,H28C), C42(H42A,H42B,
 H42C), C35(H35A,H35B,H35C), C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C49(H49A,
 H49B,H49C)
;
_shelx_res_checksum              93422
_olex2_exptl_crystal_mounting_method
'crystal mounted with the gum on glass fiber tip at room temparature'
_olex2_submission_original_sample_id gnrg-vb119
_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 1.267
_oxdiff_exptl_absorpt_empirical_full_min 0.786