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_4517802
_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 Ba0.5 Cs0.5 O6), Br6 Sb1, 1.783(C3 H7 N O)'
_chemical_formula_sum            'C29.35 H60.48 Ba Br6 Cs N1.78 O13.78 Sb'
_chemical_formula_weight         1530.44
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-05-28
_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                   14.0504(3)
_cell_length_b                   14.0504(3)
_cell_length_c                   21.4176(5)
_cell_measurement_reflns_used    8037
_cell_measurement_temperature    120.01(19)
_cell_measurement_theta_max      30.1870
_cell_measurement_theta_min      2.5290
_cell_volume                     3661.67(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(19)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0839
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -83.00   3.00   1.00   25.00    --  -25.15 -77.00  60.00   86
  2  \w    -91.00 -48.00   1.00   25.00    --  -25.15 142.00  52.37   43
  3  \w    -94.00   3.00   1.00   25.00    --  -25.15 -77.00-120.00   97
  4  \w    -47.00  44.00   1.00   25.00    --  -25.15  38.00-120.00   91
  5  \w    -93.00  -8.00   1.00   25.00    --  -25.15 -57.00 -30.00   85
  6  \w    -90.00  -7.00   1.00   25.00    --  -25.15 -57.00 120.00   83
  7  \w    -91.00  -8.00   1.00   25.00    --  -25.15 142.00-137.59   83
  8  \w     20.00  94.00   1.00   25.00    --   25.62   0.00-120.00   74
  9  \w     32.00 100.00   1.00   25.00    --   25.62-179.00 120.00   68
 10  \w    -46.00  -1.00   1.00   25.00    --   25.62   0.00-120.00   45
 11  \w    -43.00  52.00   1.00   25.00    --   25.62 -19.00  60.00   95
;
_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      -0.0213486000
_diffrn_orient_matrix_UB_12      -0.0443449000
_diffrn_orient_matrix_UB_13      0.0214701000
_diffrn_orient_matrix_UB_21      0.0273742000
_diffrn_orient_matrix_UB_22      -0.0233977000
_diffrn_orient_matrix_UB_23      -0.0162636000
_diffrn_orient_matrix_UB_31      0.0468197000
_diffrn_orient_matrix_UB_32      0.0296314000
_diffrn_orient_matrix_UB_33      0.0192845000
_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  0.0464
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            26387
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.502
_diffrn_reflns_theta_min         1.925
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    7.055
_exptl_absorpt_correction_T_max  0.47720
_exptl_absorpt_correction_T_min  0.46451
_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 yellowish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.082
_exptl_crystal_description       sphere
_exptl_crystal_F_000             2194
_exptl_crystal_recrystallization_method 'crystallized from dimethylformamide'
_exptl_crystal_size_max          0.208
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.071
_exptl_crystal_size_rad          0.075
_refine_diff_density_max         0.877
_refine_diff_density_min         -0.894
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.182
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     82
_refine_ls_number_reflns         2495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.182
_refine_ls_R_factor_all          0.0485
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0171P)^2^+33.9898P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0769
_refine_ls_wR_factor_ref         0.0802
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2127
_reflns_number_total             2495
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1998033.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4517797--4517805.cif.'
_cod_original_cell_volume        3661.69(19)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4517802
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cs Ba C36 H72 O18 Sb Br6'
_shelx_estimated_absorpt_t_max   0.634
_shelx_estimated_absorpt_t_min   0.322
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_olex2_refinement_description
;
1. 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
2. Shared sites
{Cs1, Ba1}
3. Uiso/Uaniso restraints and constraints
Uanis(C5) = Uanis(O3) = Uanis(N1) = Uanis(C7) = Uanis(C6)
Uanis(Ba1) = Uanis(Cs1)
4. Others
 Sof(O3)=Sof(N1)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=
 Sof(H7A)=Sof(H7B)=Sof(H7C)=FVAR(1)
 Fixed Sof: Ba1(0.16667) Cs1(0.16667)
5.a Free rotating group:
 O3(N1,C5,C6,C7)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B)
5.c Me refined with riding coordinates:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C)
5.d Aromatic/amide H refined with riding coordinates:
 C5(H5)
;
_shelx_res_checksum              36550
_shelx_hkl_checksum              11877
_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 1.288
_oxdiff_exptl_absorpt_empirical_full_min 0.824