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_7249125
_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 Se'
_chemical_formula_sum            'C12 H25 K O10 Se'
_chemical_formula_weight         447.38
_chemical_name_systematic        Cr6KHSeO4
_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             2024-04-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-04-22 deposited with the CCDC.	2024-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.137(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.3653(5)
_cell_length_b                   8.5649(6)
_cell_length_c                   21.5820(14)
_cell_measurement_reflns_used    1340
_cell_measurement_temperature    298
_cell_measurement_theta_max      19.4350
_cell_measurement_theta_min      2.0730
_cell_volume                     1886.1(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.85a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298
_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 0.826
_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    -39.00   9.00   1.00  385.00    --  -16.52 -77.00-180.00   48
  2  \w    -73.00  54.00   1.00  385.00    --  -16.52   0.00 120.00  127
  3  \w      1.00  51.00   1.00  385.00    --   17.46 -99.00 150.00   50
;
_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      -0.0115338000
_diffrn_orient_matrix_UB_12      -0.0794342000
_diffrn_orient_matrix_UB_13      -0.0085166000
_diffrn_orient_matrix_UB_21      0.0014235000
_diffrn_orient_matrix_UB_22      0.0189958000
_diffrn_orient_matrix_UB_23      -0.0318590000
_diffrn_orient_matrix_UB_31      0.0685349000
_diffrn_orient_matrix_UB_32      -0.0137568000
_diffrn_orient_matrix_UB_33      0.0051837000
_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  0.0677
_diffrn_reflns_av_unetI/netI     0.1562
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.826
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            8987
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.826
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.322
_diffrn_reflns_theta_min         1.917
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.256
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58438
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.85a (Rigaku Oxford Diffraction, 2023)
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    1.576
_exptl_crystal_description       needle
_exptl_crystal_F_000             920
_exptl_crystal_preparation       solution
_exptl_crystal_recrystallization_method 'slow evaporation'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         4269
_refine_ls_number_restraints     356
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.2256
_refine_ls_R_factor_gt           0.0998
_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^)+(0.0739P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1636
_refine_ls_wR_factor_ref         0.2103
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1856
_reflns_number_total             4269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00514g2.cif
_cod_data_source_block           K-anhydrous
_cod_depositor_comments
'Adding full bibliography for 7249122--7249126.cif.'
_cod_database_code               7249125
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C12 O10 K1 Se1 H25'
_shelx_estimated_absorpt_t_max   0.896
_shelx_estimated_absorpt_t_min   0.896
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 O8-H8
 0.85 with sigma of 0.01
 K1-C6
 3.65 with sigma of 0.02
 K1-C10
 3.65 with sigma of 0.02
 Se1-H8
 2.128801 with sigma of 0.02
 K1-H8
 3.671602 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O5, Se1, K1, O8, O7, O9, O10, O1, O3, O4, O6, O2, C6, C10, H8, C9, C8, C1,
 C12, C4, C5, C7, C11, C3, C2, H6A, H6B, H10A, H10B, H9A, H9B, H8A, H8B, H1A,
 H1B, H12A, H12B, H4A, H4B, H5A, H5B, H7A, H7B, H11A, H11B, H3A, H3B, H2A, H2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O9, Se1, K1, O8, O7, O10, O5, O1, O3, O4, O6, O2, C6, C10, H8, C9, C8, C1,
 C12, C4, C5, C7, C11, C3, C2, H6A, H6B, H10A, H10B, H9A, H9B, H8A, H8B, H1A,
 H1B, H12A, H12B, H4A, H4B, H5A, H5B, H7A, H7B, H11A, H11B, H3A, H3B, H2A, H2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, Se1, K1, O8, O7, O9, O10, O1, O6, O2, O5, O3, O4, C6, H8, C1, C12, C11,
 C3, C2, C9, C8, C4, C5, C7, H10A, H10B, H6A, H6B, H1A, H1B, H12A, H12B, H11A,
 H11B, H3A, H3B, H2A, H2B, H9A, H9B, H8A, H8B, H4A, H4B, H5A, H5B, H7A, H7B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C11(H11A,H11B), C12(H12A,H12B), C4(H4A,H4B), C3(H3A,H3B), C9(H9A,
 H9B), C7(H7A,H7B), C10(H10A,H10B), C2(H2A,H2B), C8(H8A,H8B), C6(H6A,H6B),
 C5(H5A,H5B)
;
_shelx_res_checksum              45893
_shelx_hkl_checksum              16203
_olex2_submission_original_sample_id Cr6KHSeO4_Anh
_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 1.264
_oxdiff_exptl_absorpt_empirical_full_min 0.738