Supramolecular Approach for Fine-Tuning of the Bright Luminescence from Zero-Dimensional Antimony(III) Halides
Morad, Viktoriia; Yakunin, Sergii; Kovalenko, Maksym V.; ACS Materials Letters  (2020) 845–852; doi:10.1021/acsmaterialslett.0c00174

data_4517801
_publ_section_title
;
 Supramolecular Approach for Fine-Tuning of the Bright Luminescence from
 Zero-Dimensional Antimony(III) Halides
;
_journal_name_full               'ACS Materials Letters'
_journal_page_first              845
_journal_page_last               852
_journal_paper_doi               10.1021/acsmaterialslett.0c00174
_journal_year                    2020
_chemical_formula_moiety         '2(C12 H24 Cs O6), Br6 Cs Sb'
_chemical_formula_sum            'C24 H48 Br6 Cs3 O12 Sb'
_chemical_formula_weight         1528.56
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-05-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.9947(6)
_cell_length_b                   9.10191(15)
_cell_length_c                   14.9567(3)
_cell_measurement_reflns_used    26748
_cell_measurement_temperature    120.01(18)
_cell_measurement_theta_max      32.6180
_cell_measurement_theta_min      2.5440
_cell_volume                     4355.58(14)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    OLEX2
_computing_publication_material  OLEX2
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.01(18)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0839
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.967
_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    -28.00  37.00   1.00   30.00    --  -25.31  38.00 -60.00   65
  2  \w    -42.00  44.00   1.00   30.00    --  -25.31  77.00 150.00   86
  3  \w    -99.00 -53.00   1.00   30.00    --  -25.31 155.00-131.52   46
  4  \w    -83.00  -9.00   1.00   30.00    --  -25.31 129.00  18.17   74
  5  \w    -92.00   2.00   1.00   30.00    --  -25.31 -77.00-180.00   94
  6  \w    -88.00   3.00   1.00   30.00    --  -25.31 -19.00-180.00   91
  7  \w     34.00  80.00   1.00   30.00    --   25.77 179.00  90.00   46
  8  \w     -3.00  91.00   1.00   30.00    --   25.77  77.00 -60.00   94
  9  \w      7.00  85.00   1.00   30.00    --   25.77  57.00 150.00   78
 10  \w    -11.00  66.00   1.00   30.00    --   25.77 -99.00-120.00   77
 11  \w      4.00  94.00   1.00   30.00    --   25.77  77.00  30.00   90
;
_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      -0.0020946000
_diffrn_orient_matrix_UB_12      -0.0110936000
_diffrn_orient_matrix_UB_13      0.0467240000
_diffrn_orient_matrix_UB_21      -0.0007194000
_diffrn_orient_matrix_UB_22      0.0771362000
_diffrn_orient_matrix_UB_23      0.0065985000
_diffrn_orient_matrix_UB_31      -0.0220580000
_diffrn_orient_matrix_UB_32      -0.0014509000
_diffrn_orient_matrix_UB_33      -0.0046421000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            92134
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.763
_diffrn_reflns_theta_min         2.326
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    8.656
_exptl_absorpt_correction_T_max  0.10666
_exptl_absorpt_correction_T_min  0.07395
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Spherical absorption correction
 using equivalent radius and absorption coefficient.
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    2.331
_exptl_crystal_description       sphere
_exptl_crystal_F_000             2856
_exptl_crystal_recrystallization_method
;
crystallized from dimethylformamide (solvent) 
and diethylether (antisolvent)
;
_exptl_crystal_size_max          0.919
_exptl_crystal_size_mid          0.325
_exptl_crystal_size_min          0.195
_exptl_crystal_size_rad          0.228
_refine_diff_density_max         0.904
_refine_diff_density_min         -1.157
_refine_diff_density_rms         0.160
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.494(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         15190
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0423
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0409P)^2^+8.9033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0971
_reflns_Friedel_coverage         0.888
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.917
_reflns_number_gt                13815
_reflns_number_total             15190
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1997953.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 4517797--4517805.cif.'
_cod_original_cell_volume        4355.57(14)
_cod_database_code               4517801
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cs3 Sb Br6 C24 H48 O12'
_chemical_oxdiff_usercomment     'same crystal at 120K'
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.506(14)
 0.494(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B),
 C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B),
 C12(H12A,H12B), C13(H13A,H13B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B),
  C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B)
;
_shelx_res_checksum              85329
_shelx_hkl_checksum              49849
_olex2_exptl_crystal_mounting_method tip-mounted
_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 59.330
_oxdiff_exptl_absorpt_empirical_full_min 0.463