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_4517797
_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         'C28.5 H58.5 Ba1 Br6 N1.5 O13.5 Rb1 Sb1'
_chemical_formula_sum            'C28.5 H58.5 Ba Br6 N1.5 O13.5 Rb Sb'
_chemical_formula_weight         1462.28
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                120
_cell_formula_units_Z            3
_cell_length_a                   14.0505(5)
_cell_length_b                   14.0505(5)
_cell_length_c                   21.0782(8)
_cell_measurement_reflns_used    8381
_cell_measurement_temperature    138(3)
_cell_measurement_theta_max      32.4360
_cell_measurement_theta_min      2.5560
_cell_volume                     3603.7(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28c (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28c (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28c (Rigaku OD, 2015)'
_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      138(3)
_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 0.941
_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    -33.00  -5.00   1.00   67.50    --  -25.15 -77.00-150.00   28
  2  \w    -24.00   2.00   1.00   67.50    --  -25.15 -77.00 -30.00   26
  3  \w    -53.00  44.00   1.00   67.50    --  -25.15  77.00  60.00   97
  4  \w    -88.00  -4.00   1.00   67.50    --  -25.15 -77.00 -60.00   84
  5  \w     -6.00  40.00   1.00   67.50    --  -25.15  57.00-150.00   46
  6  \w    -41.00  32.00   1.00   67.50    --   25.62 -57.00 -30.00   73
  7  \w    -25.00  66.00   1.00   67.50    --   25.62 -99.00-180.00   91
  8  \w     30.00  68.00   1.00   67.50    --   25.62  57.00 120.00   38
;
_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      0.0390078000
_diffrn_orient_matrix_UB_12      -0.0177430000
_diffrn_orient_matrix_UB_13      -0.0030234000
_diffrn_orient_matrix_UB_21      -0.0338745000
_diffrn_orient_matrix_UB_22      -0.0469925000
_diffrn_orient_matrix_UB_23      0.0186887000
_diffrn_orient_matrix_UB_31      -0.0269280000
_diffrn_orient_matrix_UB_32      -0.0295967000
_diffrn_orient_matrix_UB_33      -0.0278232000
_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  0.0212
_diffrn_reflns_av_unetI/netI     0.0237
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.941
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15370
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.897
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.708
_diffrn_reflns_theta_min         1.932
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.426
_exptl_absorpt_correction_T_max  0.91241
_exptl_absorpt_correction_T_min  0.91241
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28c (Rigaku Oxford Diffraction, 2015)
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 yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.021
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             2106
_exptl_crystal_recrystallization_method
'crystallized from dimethylformamide (solvent) with diethylether (antisolvent)'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_exptl_crystal_size_rad          0.1
_refine_diff_density_max         0.933
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.390(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         5316
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0324
_refine_ls_R_factor_gt           0.0257
_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^)+(0.0272P)^2^+7.9931P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0618
_reflns_Friedel_coverage         0.907
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.853
_reflns_number_gt                4697
_reflns_number_total             5316
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1997955.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4517797--4517805.cif.'
_cod_original_cell_volume        3603.7(3)
_cod_original_sg_symbol_H-M      'R 3'
_cod_original_formula_sum        'C28.50 H58.50 Ba Br6 N1.50 O13.50 Rb Sb'
_cod_database_code               4517797
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 H48 O12 Sb Br6 Rb Ba'
_shelx_estimated_absorpt_t_max   0.402
_shelx_estimated_absorpt_t_min   0.318
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.609(10)
 0.391(10)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
Uiso(O6) = Uiso(C12) = Uiso(N2) = Uiso(C13) = Uiso(C14)
4. Others
 Fixed Sof: O5(0.33333) N1(0.33333) C9(0.33333) H9(0.33333) C10(0.33333)
 H10B(0.33333) H10A(0.33333) H10C(0.33333) C11(0.33333) H11B(0.33333)
 H11A(0.33333) H11C(0.33333) O6(0.16667) N2(0.16667) C12(0.16667) H12(0.16667)
 C13(0.16667) H13C(0.16667) H13A(0.16667) H13B(0.16667) C14(0.16667)
 H14A(0.16667) H14C(0.16667) H14B(0.16667)
5.a Free rotating group:
 O5(N1,C9,C10,C11), O6(N2,C12,C13,C14)
5.b 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)
5.c Me refined with riding coordinates:
 C10(H10B,H10A,H10C), C11(H11B,H11A,H11C), C13(H13C,H13A,H13B), C14(H14A,H14C,
 H14B)
5.d Aromatic/amide H refined with riding coordinates:
 C9(H9), C12(H12)
;
_shelx_res_checksum              83957
_shelx_hkl_checksum              24068
_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 1.814
_oxdiff_exptl_absorpt_empirical_full_min 0.731