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_7714400
_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, Cl O4'
_chemical_formula_sum            'C21 H21 Cl O7 Te'
_chemical_formula_weight         548.43
_chemical_name_systematic        'symmetric tellurium 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     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                111.3980(10)
_cell_angle_beta                 96.8270(10)
_cell_angle_gamma                104.1250(10)
_cell_formula_units_Z            2
_cell_length_a                   10.3196(4)
_cell_length_b                   10.7682(5)
_cell_length_c                   11.1672(5)
_cell_measurement_reflns_used    9669
_cell_measurement_temperature    285
_cell_measurement_theta_max      30.37
_cell_measurement_theta_min      2.94
_cell_volume                     1090.36(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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_temperature      284.87
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0298
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            58169
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.551
_diffrn_reflns_theta_min         2.939
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.526
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6494
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1229 before and 0.0442 after correction. The Ratio of minimum to maximum transmission is 0.8704. The \l/2 correction factor is 0.00150.'
_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    1.670
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_preparation       'diffusions method'
_exptl_crystal_recrystallization_method 'diffusion method mother liquor hexane'
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     274
_refine_ls_number_reflns         6644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.0223
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0299P)^2^+0.3123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0550
_refine_ls_wR_factor_ref         0.0574
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5940
_reflns_number_total             6644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02746e2.cif
_cod_data_source_block           vb584_0m_a
_cod_database_code               7714400
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.914
_shelx_estimated_absorpt_t_min   0.875
_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:
 C19(H19), C20(H20), C5(H5), C6(H6), C11(H11), C17(H17), C12(H12), C8(H8),
 C16(H16), C3(H3), C2(H2), C9(H9)
2.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              86832
_olex2_exptl_crystal_mounting_method 'ON FIBER TIP'
_olex2_submission_original_sample_id VB584
_olex2_submission_special_instructions 'No special instructions were received'