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_7249122
_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, 2(H2 O)'
_chemical_formula_sum            'C12 H29 K O12 Se'
_chemical_formula_weight         483.41
_chemical_name_systematic        Crown6KHSeO4_2H2O
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2024-04-22 deposited with the CCDC.	2024-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.351(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4882(5)
_cell_length_b                   17.5369(5)
_cell_length_c                   8.4421(3)
_cell_measurement_reflns_used    2354
_cell_measurement_temperature    293
_cell_measurement_theta_max      25.8630
_cell_measurement_theta_min      3.6650
_cell_volume                     2110.04(12)
_computing_cell_refinement       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)'
_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      293(2)
_diffrn_detector_area_resol_mean 16.1340
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.829
_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 -13.00   1.00   30.00    --  -17.75 -77.00-180.00   26
  2  \w    -48.00  41.00   1.00   30.00    --   18.92 -19.00 -30.00   89
  3  \w    -47.00  40.00   1.00   30.00    --   18.92 -38.00-120.00   87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0581
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.829
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4271
_diffrn_reflns_point_group_measured_fraction_full 0.635
_diffrn_reflns_point_group_measured_fraction_max 0.512
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.249
_diffrn_reflns_theta_min         3.379
_exptl_absorpt_coefficient_mu    2.030
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.67828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022)
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    1.522
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_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         0.768
_refine_diff_density_min         -0.368
_refine_diff_density_rms         0.096
_refine_ls_abs_structure_details
;
 Flack x determined using 466 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.029(16)
_refine_ls_extinction_coef       0.0107(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         2952
_refine_ls_number_restraints     311
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0880P)^2^+1.1518P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1402
_refine_ls_wR_factor_ref         0.1453
_reflns_Friedel_coverage         0.233
_reflns_Friedel_fraction_full    0.271
_reflns_Friedel_fraction_max     0.194
_reflns_number_gt                2513
_reflns_number_total             2952
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00514g2.cif
_cod_data_source_block           K-hydrated
_cod_depositor_comments
'Adding full bibliography for 7249122--7249126.cif.'
_cod_database_code               7249122
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.905
_shelx_estimated_absorpt_t_min   0.905
_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, All O(H,H) groups
2. Restrained distances
 O7-H7
 0.85 with sigma of 0.01
 Se01-H7
 2.037497 with sigma of 0.02
 K1-H7
 3.679595 with sigma of 0.02
3. Rigid body (RIGU) restrains
 K1, Se01, O10, O8, O9, O7, O4, O2, O6, O3, O5, O1, H7, C7, C6, C2, C3, C11,
 C10, C5, C4, C8, C9, C12, C1, H7A, H7B, H6A, H6B, H2A, H2B, H3A, H3B, H11A,
 H11B, H10A, H10B, H5A, H5B, H4A, H4B, H8A, H8B, H9A, H9B, H12A, H12B, H1A, H1B,
  O11, H11C, H11D, O12, H12C, H12D
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Everything fixed:
 O12, H12C, H12D, H11C, H11D
4.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C1(H1A,H1B), C2(H2A,H2B), C5(H5A,H5B), C8(H8A,H8B), C11(H11A,
 H11B), C9(H9A,H9B), C4(H4A,H4B), C7(H7A,H7B), C10(H10A,H10B), C3(H3A,H3B),
 C6(H6A,H6B)
;
_shelx_res_checksum              35697
_shelx_hkl_checksum              11502
_olex2_submission_original_sample_id Cr6KHSeO4
_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
;