Potassium-telluroether interactions: structural characterisation and computational analysis.
Gray, Novan A. G.; Britten, James F.; Emslie, David J. H.; Chemical communications (Cambridge, England) 61 (2025) 3143–3146; doi:10.1039/d4cc06539e

data_7134197
_publ_section_title
;
 Potassium-telluroether interactions: structural characterisation and
 computational analysis.
;
_journal_issue                   15
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3143
_journal_page_last               3146
_journal_paper_doi               10.1039/d4cc06539e
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C59 H86 K N O3 Te2'
_chemical_formula_sum            'C59 H86 K N O3 Te2'
_chemical_formula_weight         1151.58
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-09 deposited with the CCDC.	2025-01-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.362(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.372(4)
_cell_length_b                   18.509(10)
_cell_length_c                   32.590(16)
_cell_measurement_reflns_used    8365
_cell_measurement_temperature    112.00
_cell_measurement_theta_max      21.85
_cell_measurement_theta_min      2.45
_cell_volume                     5618(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      112.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1750
_diffrn_reflns_av_unetI/netI     0.0813
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            173803
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.130
_diffrn_reflns_theta_min         2.448
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.155
_exptl_absorpt_correction_T_max  0.7263
_exptl_absorpt_correction_T_min  0.6614
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1089 before and 0.0826 after correction.
The Ratio of minimum to maximum transmission is 0.9106.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       block
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.255
_refine_diff_density_min         -1.123
_refine_diff_density_rms         0.135
_refine_ls_extinction_coef       0.00055(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         15112
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0982
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0467P)^2^+13.0513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1164
_refine_ls_wR_factor_ref         0.1376
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9982
_reflns_number_total             15112
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06539e3.cif
_cod_data_source_block           KTeNTeTrippTHF3
_cod_depositor_comments
'Adding full bibliography for 7134197--7134200.cif.'
_cod_original_cell_volume        5619(5)
_cod_database_code               7134197
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.874
_olex2_refinement_description
;
1. Restrained distances
 C54-C53 \\sim C61-C60 \\sim C50-C49
 with sigma of 0.02
 C61-C55 \\sim C55-C54 \\sim C60-C52 \\sim C53-C52 \\sim C48-C49
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(C61) = Uanis(C60)
Uanis(C54) = Uanis(C53)
3. Others
 Fixed Sof: H52A(0.5) H52B(0.5) H52C(0.5) H52D(0.5) H55A(0.5) H55B(0.5)
 H55C(0.5) H55D(0.5) C61(0.5) H61A(0.5) H61B(0.5) C60(0.5) H60A(0.5) H60B(0.5)
 C53(0.5) H53A(0.5) H53B(0.5) C54(0.5) H54A(0.5) H54B(0.5)
4.a Ternary CH refined with riding coordinates:
 C30(H30), C42(H42), C24(H24), C39(H39), C45(H45), C27(H27)
4.b Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C59(H59A,H59B), C49(H49A,H49B), C48(H48A,H48B), C52(H52A,
 H52B), C52(H52C,H52D), C58(H58A,H58B), C50(H50A,H50B), C51(H51A,H51B),
 C57(H57A,H57B), C55(H55A,H55B), C55(H55C,H55D), C61(H61A,H61B), C60(H60A,H60B),
  C53(H53A,H53B), C54(H54A,H54B)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C11(H11), C5(H5), C9(H9), C35(H35), C22(H22), C37(H37), C20(H20)
4.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C15(H15A,H15B,
 H15C), C26(H26A,H26B,H26C), C46(H46A,H46B,H46C), C25(H25A,H25B,H25C), C41(H41A,
 H41B,H41C), C47(H47A,H47B,H47C), C32(H32A,H32B,H32C), C31(H31A,H31B,H31C),
 C44(H44A,H44B,H44C), C43(H43A,H43B,H43C), C40(H40A,H40B,H40C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              76444
_shelx_hkl_checksum              2444
_olex2_submission_special_instructions 'No special instructions were received'