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_7249124
_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 O10 Rb Se, H2 O'
_chemical_formula_sum            'C12 H27 O11 Rb Se'
_chemical_formula_weight         511.76
_chemical_name_systematic        Crown6RbHSeO4_H2O
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-02-07
_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                 117.183(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.1681(14)
_cell_length_b                   9.9047(4)
_cell_length_c                   20.5896(12)
_cell_measurement_reflns_used    1827
_cell_measurement_temperature    293
_cell_measurement_theta_max      23.5730
_cell_measurement_theta_min      3.4460
_cell_volume                     4021.5(5)
_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
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1340
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.840
_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    -87.00 -51.00   1.00  135.00    --  -17.60-178.00-150.00   36
  2  \w    -28.00  33.00   1.00  135.00    --  -17.60  77.00   0.00   61
  3  \w    -25.00  77.00   1.00  135.00    --   18.92  19.00-180.00  102
;
_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      -0.0295223000
_diffrn_orient_matrix_UB_12      -0.0011577000
_diffrn_orient_matrix_UB_13      0.0051390000
_diffrn_orient_matrix_UB_21      0.0140577000
_diffrn_orient_matrix_UB_22      -0.0534425000
_diffrn_orient_matrix_UB_23      0.0255117000
_diffrn_orient_matrix_UB_31      0.0149815000
_diffrn_orient_matrix_UB_32      0.0477043000
_diffrn_orient_matrix_UB_33      0.0286626000
_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  0.0534
_diffrn_reflns_av_unetI/netI     0.1169
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.840
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            8182
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.840
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         29.071
_diffrn_reflns_theta_min         3.453
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.321
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92297
_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    1.691
_exptl_crystal_description       plate
_exptl_crystal_F_000             2064
_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         0.395
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         4533
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      0.997
_refine_ls_R_factor_all          0.1335
_refine_ls_R_factor_gt           0.0502
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0741
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2260
_reflns_number_total             4533
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00514g2.cif
_cod_data_source_block           Rb-hydrated
_cod_depositor_comments
'Adding full bibliography for 7249122--7249126.cif.'
_cod_database_code               7249124
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C12 O10 Se1 Rb1 H25'
_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
 O00A-H00A
 0.85 with sigma of 0.01
 C00F-Rb01
 3.7 with sigma of 0.02
 Rb01-C00F
 3.72 with sigma of 0.02
 Rb01-C00K
 3.8 with sigma of 0.02
 C00K-Rb01
 3.8 with sigma of 0.02
 Rb01_$1-H00A
 3.68 with sigma of 0.02
 H00A-O00B_$1
 1.73 with sigma of 0.02
 Se02-H00A
 2 with sigma of 0.02
 H00A-Se02
 2.2 with sigma of 0.02
 Se02-H00A
 2.139972 with sigma of 0.02
 Rb01-H00A
 4.370042 with sigma of 0.02
3.a Free rotating group:
 O00N(H00Z,H)
3.b Secondary CH2 refined with riding coordinates:
 C00D(H00B,H00C), C00E(H00D,H00E), C00F(H00F,H00G), C00G(H00H,H00I), C00H(H00J,
 H00K), C00I(H00L,H00M), C00J(H00N,H00O), C00K(H00P,H00Q), C00L(H00R,H00S),
 C00M(H00T,H00U), C00O(H00V,H00W), C00P(H00X,H00Y)
;
_shelx_res_checksum              48476
_shelx_hkl_checksum              91517
_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 1.057
_oxdiff_exptl_absorpt_empirical_full_min 0.940