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_7134200
_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 Se2, C6 H14'
_chemical_formula_sum            'C65 H100 K N O3 Se2'
_chemical_formula_weight         1140.47
_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             2024-07-23
_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                 95.108(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.312(5)
_cell_length_b                   18.550(9)
_cell_length_c                   35.565(16)
_cell_measurement_reflns_used    8334
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      19.94
_cell_measurement_theta_min      2.20
_cell_volume                     6119(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      100.00
_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  0.1788
_diffrn_reflns_av_unetI/netI     0.1472
_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       -9
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            112942
_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         28.282
_diffrn_reflns_theta_min         2.045
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.320
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6499
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1080 before and 0.0790 after correction.
The Ratio of minimum to maximum transmission is 0.8711.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       plate
_exptl_crystal_F_000             2432
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.322
_refine_diff_density_min         -3.083
_refine_diff_density_rms         0.216
_refine_ls_extinction_coef       0.0017(4)
_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   1.180
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     651
_refine_ls_number_reflns         15183
_refine_ls_number_restraints     636
_refine_ls_restrained_S_all      1.158
_refine_ls_R_factor_all          0.2331
_refine_ls_R_factor_gt           0.1717
_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^)+(0.0595P)^2^+213.0341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3846
_refine_ls_wR_factor_ref         0.4110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9483
_reflns_number_total             15183
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc06539e3.cif
_cod_data_source_block           KSeNSeTrippTHF3
_cod_depositor_comments
'Adding full bibliography for 7134197--7134200.cif.'
_cod_database_code               7134200
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.961
_shelx_estimated_absorpt_t_min   0.778
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.938(3)
 0.062(3)
2. 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
3. Uiso/Uaniso restraints and constraints
Uanis(C20) = Uanis(C22)
Uanis(C6) = Uanis(C8)
Uanis(C15) = Uanis(C16)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C30(H30), C39(H39), C24(H24), C27(H27), C42(H42), C45(H45)
5.b Secondary CH2 refined with riding coordinates:
 C56(H56A,H56B), C49(H49A,H49B), C48(H48A,H48B), C54(H54A,H54B), C53(H53A,
 H53B), C52(H52A,H52B), C55(H55A,H55B), C58(H58A,H58B), C50(H50A,H50B),
 C51(H51A,H51B), C62(H62A,H62B), C59(H59A,H59B), C57(H57A,H57B), C61(H61A,H61B),
  C63(H63A,H63B), C64(H64A,H64B)
5.c Aromatic/amide H refined with riding coordinates:
 C37(H37), C5(H5), C11(H11), C9(H9), C22(H22), C3(H3), C20(H20), C35(H35)
5.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C15(H15A,H15B,H15C), C14(H14A,H14B,
 H14C), C32(H32A,H32B,H32C), C47(H47A,H47B,H47C), C43(H43A,H43B,H43C), C41(H41A,
 H41B,H41C), C25(H25A,H25B,H25C), C44(H44A,H44B,H44C), C26(H26A,H26B,H26C),
 C46(H46A,H46B,H46C), C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C31(H31A,H31B,
 H31C), C40(H40A,H40B,H40C), C60(H60A,H60B,H60C), C65(H65A,H65B,H65C)
;
_shelx_res_checksum              58258
_shelx_hkl_checksum              76495
_olex2_submission_special_instructions 'No special instructions were received'