Effect of supramolecular complexation of alkali hydrogenselenates with crown ethers and solid-solutions with their hydrogensulfate counterparts on the solid-to-solid phase transition behaviors
Ocak, Samet; Braga, Dario; d'Agostino, Simone; CrystEngComm 26 (2024) 4525–4532; doi:10.1039/D4CE00514G

data_7249123
_publ_section_title
;
 Effect of supramolecular complexation of alkali hydrogenselenates with
 crown ethers and solid-solutions with their hydrogensulfate counterparts
 on the solid-to-solid phase transition behaviors
;
_journal_issue                   33
_journal_name_full               CrystEngComm
_journal_page_first              4525
_journal_page_last               4532
_journal_paper_doi               10.1039/D4CE00514G
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C12 H25 K O10 S0.5 Se0.5'
_chemical_formula_sum            'C12 H25 K O10 S0.5 Se0.5'
_chemical_formula_weight         423.93
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-16
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-04-22 deposited with the CCDC.	2024-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.684(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3093(8)
_cell_length_b                   8.5230(6)
_cell_length_c                   21.5977(15)
_cell_measurement_reflns_used    956
_cell_measurement_temperature    295
_cell_measurement_theta_max      19.5320
_cell_measurement_theta_min      2.0720
_cell_volume                     1870.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 42.85a 64-bit (release 03-03-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.117a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      295
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1385
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.825
_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  15.00   1.00  125.00    --  -16.52 -19.00-120.00   66
  2  \w    -33.00  88.00   1.00  125.00    --   17.46   0.00 -30.00  121
  3  \w     63.00  90.00   1.00  125.00    --   17.46 178.00 150.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0555814000
_diffrn_orient_matrix_UB_12      0.0476209000
_diffrn_orient_matrix_UB_13      0.0019314000
_diffrn_orient_matrix_UB_21      0.0149722000
_diffrn_orient_matrix_UB_22      0.0473670000
_diffrn_orient_matrix_UB_23      -0.0248796000
_diffrn_orient_matrix_UB_31      -0.0395002000
_diffrn_orient_matrix_UB_32      -0.0490776000
_diffrn_orient_matrix_UB_33      -0.0220887000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0719
_diffrn_reflns_av_unetI/netI     0.2040
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.825
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            8510
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.825
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.521
_diffrn_reflns_theta_min         2.070
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.358
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96077
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.117a (Rigaku Oxford Diffraction, 2024)
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    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             884
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.214
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     268
_refine_ls_number_reflns         4312
_refine_ls_number_restraints     471
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.2703
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0375P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1083
_refine_ls_wR_factor_ref         0.1624
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1396
_reflns_number_total             4312
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00514g2.cif
_cod_data_source_block           K-Se-S_sol-sod
_cod_depositor_comments
'Adding full bibliography for 7249122--7249126.cif.'
_cod_original_formula_sum        'C12 H25 K O10 S0.50 Se0.50'
_cod_database_code               7249123
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C12 O10 S0.5 Se0.5 K1 H25 '
_shelx_estimated_absorpt_t_max   0.960
_shelx_estimated_absorpt_t_min   0.935
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O006-H006
 0.85 with sigma of 0.01
 O11-H11
 0.85 with sigma of 0.01
 Se1-H006
 2.072321 with sigma of 0.02
 K002-H006
 3.612806 with sigma of 0.02
 S1-H11
 1.969188 with sigma of 0.02
 K002-H11
 3.688742 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C1, H1A, H1B, C2, O6, H2A, H2B, O1, C12, K002, C3, C11, H12A, H12B, O5, O13,
 O3, O12, O006, O11, O4, O2, Se1, S1, H3A, H3B, C4, H11A, H11B, C10, C6, C7,
 H006, H11, C8, C9, C5, O8, O9, O7, O10, H4A, H4B, H10A, H10B, H6A, H6B, H7A,
 H7B, H8A, H8B, H9A, H9B, H5A, H5B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O006(0.5) H006(0.5) O7(0.5) O8(0.5) O9(0.5) O10(0.5) O11(0.5)
 H11(0.5) O12(0.5) O13(0.5) S1(0.5) Se1(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B)
;
_shelx_res_checksum              87957
_shelx_hkl_checksum              33190
_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 1.084
_oxdiff_exptl_absorpt_empirical_full_min 0.938