Attractive and repulsive forces in a crystal of [Rb(18-crown-6)][SbCl<sub>6</sub>] under high pressure.
Rusanov, Eduard B.; Wörle, Michael D; Kovalenko, Maksym V.; Domasevitch, Kostiantyn V.; Rusanova, Julia A.; Acta crystallographica Section B, Structural science, crystal engineering and materials 80 (2024) 135–145; doi:10.1107/S2052520624001586

data_2312451
_publ_section_title
;
 Attractive and repulsive forces in a crystal of
 [Rb(18-crown-6)][SbCl<sub>6</sub>] under high pressure.
;
_journal_issue                   'Pt 2'
_journal_name_full
'Acta crystallographica Section B, Structural science, crystal engineering and materials'
_journal_page_first              135
_journal_page_last               145
_journal_paper_doi               10.1107/S2052520624001586
_journal_volume                  80
_journal_year                    2024
_chemical_formula_moiety         'C12 H24 O6 Rb, Cl6 Sb'
_chemical_formula_sum            'C12 H24 Cl6 O6 Rb Sb'
_chemical_formula_weight         684.23
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-12-19
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   13.7392(7)
_cell_length_b                   13.7392(7)
_cell_length_c                   9.5341(6)
_cell_measurement_pressure       1610000
_cell_measurement_reflns_used    1409
_cell_measurement_temperature    293(1)
_cell_measurement_theta_max      30.0070
_cell_measurement_theta_min      2.7280
_cell_volume                     1558.59(15)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (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 2018/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_pressure         1610000
_diffrn_ambient_temperature      293(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.734
_diffrn_measured_fraction_theta_max 0.693
_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    -47.00 -22.00   1.00    3.00    --  -26.20   6.00-150.00   25
  2  \w     28.00  53.00   1.00    3.00    --  -26.20  26.00 -82.00   25
  3  \w    -34.00  -9.00   1.00    3.00    --  -26.20  77.00 -30.00   25
  4  \w    -83.00 -58.00   1.00    3.00    --  -26.20 125.00 -22.00   25
  5  \w    -93.00 -68.00   1.00    3.00    --  -26.20 147.00 143.00   25
  6  \w     -9.00  16.00   1.00    3.00    --   24.80  67.00 157.00   25
  7  \w      7.00  32.00   1.00    3.00    --   24.80  54.00 105.00   25
  8  \w     15.00  40.00   1.00    3.00    --   24.80  29.00 119.00   25
  9  \w    -34.00   3.00   1.00    3.00    --   24.80   6.00-150.00   37
 10  \w    -63.00 -37.00   1.00    3.00    --   24.80  -6.00  32.00   26
 11  \w    -32.00   3.00   1.00    3.00    --   24.80  97.00 -35.00   35
 12  \w     63.00 102.00   1.00    3.00    --   24.80 178.00 -90.00   39
 13  \w     24.00  49.00   1.00    3.00    --   24.80-125.00-100.00   25
 14  \w     43.00  68.00   1.00    3.00    --   24.80-147.00  93.00   25
 15  \w      6.00  31.00   1.00    3.00    --  -26.20 -40.00  12.00   25
 16  \w    -36.00  -4.00   1.00    3.00    --  -26.20 -13.00   3.00   32
 17  \w   -115.00 -90.00   1.00    3.00    --  -26.20 -26.00 114.00   25
 18  \w    -20.00   5.00   1.00    3.00    --  -26.20 -19.00-180.00   25
 19  \w      6.00  31.00   1.00    3.00    --  -26.20 -97.00-143.00   25
 20  \w      5.00  35.00   1.00    3.00    --  -26.20-114.00-135.00   30
 21  \w      5.00  31.00   1.00    3.00    --  -26.20-114.00  45.00   26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'diamond anvil cell'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0324980000
_diffrn_orient_matrix_UB_12      -0.0518614000
_diffrn_orient_matrix_UB_13      0.0353472000
_diffrn_orient_matrix_UB_21      -0.0215463000
_diffrn_orient_matrix_UB_22      -0.0271767000
_diffrn_orient_matrix_UB_23      -0.0652313000
_diffrn_orient_matrix_UB_31      0.0450851000
_diffrn_orient_matrix_UB_32      -0.0110306000
_diffrn_orient_matrix_UB_33      -0.0056549000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.734
_diffrn_reflns_Laue_measured_fraction_max 0.693
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2658
_diffrn_reflns_point_group_measured_fraction_full 0.734
_diffrn_reflns_point_group_measured_fraction_max 0.693
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.432
_diffrn_reflns_theta_min         2.738
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.453
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.187
_exptl_crystal_description       prizm
_exptl_crystal_F_000             1002
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         550
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0336
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0349P)^2^+0.7250P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0628
_refine_ls_wR_factor_ref         0.0646
_reflns_Friedel_coverage         0.000
_reflns_number_gt                488
_reflns_number_total             550
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            px5059.cif
_cod_data_source_block           Rb16k1
_cod_depositor_comments
'Adding full bibliography for 2312438--2312457.cif.'
_cod_original_cell_volume        1558.58(19)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2312451
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C12H24O6RbSbCl6
_chemical_oxdiff_usercomment     'RbCrSbCl6 at 16k1'
_shelx_estimated_absorpt_t_max   0.640
_shelx_estimated_absorpt_t_min   0.555
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Others
 Fixed Sof: Rb1(0.166667)
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
;
_shelx_res_checksum              11481
_shelx_hkl_checksum              4673
_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 1.513
_oxdiff_exptl_absorpt_empirical_full_min 0.794