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_7249126
_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 H24 Cs O11 Se'
_chemical_formula_sum            'C12 H24 Cs O11 Se'
_chemical_formula_weight         556.18
_chemical_name_systematic        Cr6CsHSeO4_H2O
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2024-02-06
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-22 deposited with the CCDC.	2024-07-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.486(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.7101(16)
_cell_length_b                   8.4597(7)
_cell_length_c                   21.3553(18)
_cell_measurement_reflns_used    1090
_cell_measurement_temperature    300
_cell_measurement_theta_max      20.7300
_cell_measurement_theta_min      2.2260
_cell_volume                     4038.1(6)
_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 1.5 (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      300
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1385
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.837
_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     -3.00  51.00   1.00  105.00    --  -16.52  38.00-120.00   54
  2  \w    -86.00   6.00   1.00  105.00    --  -16.52 -38.00  60.00   92
  3  \w     -7.00  18.00   1.00  105.00    --   17.30  77.00  90.00   25
  4  \w     10.00  56.00   1.00  105.00    --   17.30 -99.00-180.00   46
;
_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      -0.0025662000
_diffrn_orient_matrix_UB_12      -0.0438046000
_diffrn_orient_matrix_UB_13      -0.0291582000
_diffrn_orient_matrix_UB_21      0.0062399000
_diffrn_orient_matrix_UB_22      0.0693589000
_diffrn_orient_matrix_UB_23      -0.0151784000
_diffrn_orient_matrix_UB_31      0.0309916000
_diffrn_orient_matrix_UB_32      -0.0175527000
_diffrn_orient_matrix_UB_33      0.0126677000
_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  0.1111
_diffrn_reflns_av_unetI/netI     0.4332
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.837
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8935
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.837
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.182
_diffrn_reflns_theta_min         1.822
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.685
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75999
_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    1.830
_exptl_crystal_description       plate
_exptl_crystal_F_000             2184
_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         0.943
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.809
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4576
_refine_ls_number_restraints     304
_refine_ls_restrained_S_all      0.798
_refine_ls_R_factor_all          0.2828
_refine_ls_R_factor_gt           0.0794
_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^)+(0.0625P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1888
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1224
_reflns_number_total             4576
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 177.2725\% 
around [-0.01 1.00 0.00] (reciprocal) or [-0.00 1.00 -0.00] (direct)
;
_cod_data_source_file            d4ce00514g2.cif
_cod_data_source_block           Cs-hydrated
_cod_depositor_comments
'Adding full bibliography for 7249122--7249126.cif.'
_cod_database_code               7249126
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C12 O10 Se1 Cs1'
_shelx_estimated_absorpt_t_max   0.837
_shelx_estimated_absorpt_t_min   0.837
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 C4-Cs1
 3.95 with sigma of 0.02
 Cs1-C4
 4 with sigma of 0.02
 C5-Cs1
 4 with sigma of 0.02
 Cs1-C8
 3.9 with sigma of 0.02
3. Rigid body (RIGU) restrains
 O7, Se1, O10, O8, O9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C8, Cs1, O2, O4, O6, O1, O3, O5, C1, C9, C3, C2, C6, C7, C10, C11, C12, C5, C4
 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:
 C3(H3A,H3B), C11(H11A,H11B), C6(H6A,H6B), C5(H5A,H5B), C1(H1A,H1B), C2(H2A,
 H2B), C12(H12A,H12B), C4(H4A,H4B), C10(H10A,H10B), C7(H7A,H7B), C9(H9A,H9B),
 C8(H8A,H8B)
;
_shelx_res_checksum              38464
_shelx_hkl_checksum              51633
_olex2_submission_original_sample_id Cr6CsSe
_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 1.227
_oxdiff_exptl_absorpt_empirical_full_min 0.879
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2