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_2312444
_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                   13.9423(7)
_cell_length_b                   13.9423(7)
_cell_length_c                   9.8301(6)
_cell_measurement_pressure       680000
_cell_measurement_reflns_used    1447
_cell_measurement_temperature    293(1)
_cell_measurement_theta_max      29.7660
_cell_measurement_theta_min      2.6560
_cell_volume                     1654.85(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         680000
_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 0.729
_diffrn_measured_fraction_theta_max 0.680
_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    -36.00   8.00   1.00    4.00    --   24.80  -6.00  27.00   44
  2  \w     25.00  50.00   1.00    4.00    --   24.80-125.00-101.00   25
  3  \w     78.00 107.00   1.00    4.00    --   24.80-178.00  90.00   29
  4  \w     44.00  69.00   1.00    4.00    --   24.80-148.00  93.00   25
  5  \w      5.00  39.00   1.00    4.00    --  -26.20-114.00  45.00   34
  6  \w    -42.00 -17.00   1.00    4.00    --  -26.20  -6.00  27.00   25
  7  \w     23.00  53.00   1.00    4.00    --   24.80  55.00 104.00   30
  8  \w     15.00  40.00   1.00    4.00    --   24.80  29.00 119.00   25
  9  \w    -37.00 -15.00   1.00    4.00    --   24.80  38.00   0.00   22
 10  \w    -18.00   9.00   1.00    4.00    --   24.80  67.00 -23.00   27
 11  \w     42.00  67.00   1.00    4.00    --   24.80  25.00 -83.00   25
 12  \w    -11.00  14.00   1.00    4.00    --  -26.20 -82.00-151.00   25
 13  \w    -40.00 -14.00   1.00    4.00    --   24.80   6.00-156.00   26
 14  \w    -53.00 -11.00   1.00    4.00    --  -26.20   6.00-156.00   42
 15  \w     30.00  56.00   1.00    4.00    --  -26.20  25.00 -83.00   26
 16  \w   -114.00 -89.00   1.00    4.00    --  -26.20 178.00 -90.00   25
 17  \w    -83.00 -58.00   1.00    4.00    --  -26.20 125.00 -22.00   25
 18  \w    -94.00 -69.00   1.00    4.00    --  -26.20 148.00 142.00   25
;
_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      0.0189028000
_diffrn_orient_matrix_UB_12      0.0512485000
_diffrn_orient_matrix_UB_13      -0.0339445000
_diffrn_orient_matrix_UB_21      0.0050536000
_diffrn_orient_matrix_UB_22      0.0264716000
_diffrn_orient_matrix_UB_23      0.0633524000
_diffrn_orient_matrix_UB_31      0.0554135000
_diffrn_orient_matrix_UB_32      0.0112936000
_diffrn_orient_matrix_UB_33      0.0057996000
_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  0.0283
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.729
_diffrn_reflns_Laue_measured_fraction_max 0.680
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2343
_diffrn_reflns_point_group_measured_fraction_full 0.729
_diffrn_reflns_point_group_measured_fraction_max 0.680
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         2.672
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    4.194
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.34541
_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    2.060
_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         0.277
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         577
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0297
_refine_ls_R_factor_gt           0.0248
_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^)+(0.0326P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0571
_refine_ls_wR_factor_ref         0.0591
_reflns_Friedel_coverage         0.000
_reflns_number_gt                519
_reflns_number_total             577
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            px5059.cif
_cod_data_source_block           Rb6k8
_cod_depositor_comments
'Adding full bibliography for 2312438--2312457.cif.'
_cod_original_cell_volume        1654.84(19)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               2312444
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C12H24O6RbSbCl6
_chemical_oxdiff_usercomment     'RbCrSbCl6 at 6k8'
_shelx_estimated_absorpt_t_max   0.655
_shelx_estimated_absorpt_t_min   0.572
_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              7963
_shelx_hkl_checksum              98986
_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 2.498
_oxdiff_exptl_absorpt_empirical_full_min 0.781