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_4517803
_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
'C30 H62 Ba2 Br6 N2 O14 Sb, C1.5 H3.5 Br4 N0.5 O0.5 Sb'
_chemical_formula_sum            'C31.5 H65.5 Ba2 Br10 N2.5 O14.5 Sb2'
_chemical_formula_weight         2028.64
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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                80.825(2)
_cell_angle_beta                 86.605(2)
_cell_angle_gamma                89.767(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9339(2)
_cell_length_b                   13.8500(4)
_cell_length_c                   24.0142(7)
_cell_measurement_reflns_used    13223
_cell_measurement_temperature    200.01(12)
_cell_measurement_theta_max      31.2220
_cell_measurement_theta_min      2.0830
_cell_volume                     2928.18(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      200.01(12)
_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    -70.00  -8.00   1.00  100.00    --  -24.99   0.00 150.00   62
  2  \w    -28.00  46.00   1.00  100.00    --  -24.99  38.00-180.00   74
  3  \w      0.00  94.00   1.00  100.00    --   25.46  77.00 150.00   94
  4  \w     -3.00  95.00   1.00  100.00    --   25.46  77.00 -90.00   98
  5  \w    -22.00  66.00   1.00  100.00    --   25.46 -99.00-120.00   88
  6  \w      7.00  83.00   1.00  100.00    --   25.46  57.00  90.00   76
  7  \w      4.00  79.00   1.00  100.00    --   25.46-123.00 127.00   75
  8  \w    -43.00  41.00   1.00  100.00    --   25.46 -77.00 -60.00   84
  9  \w    -24.00  66.00   1.00  100.00    --   25.46 -99.00  30.00   90
 10  \w      7.00  86.00   1.00  100.00    --   25.46  57.00  30.00   79
;
_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      -0.0140735000
_diffrn_orient_matrix_UB_12      0.0021946000
_diffrn_orient_matrix_UB_13      0.0291508000
_diffrn_orient_matrix_UB_21      -0.0623169000
_diffrn_orient_matrix_UB_22      0.0308221000
_diffrn_orient_matrix_UB_23      -0.0064041000
_diffrn_orient_matrix_UB_31      -0.0473740000
_diffrn_orient_matrix_UB_32      -0.0416711000
_diffrn_orient_matrix_UB_33      0.0027498000
_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  0.0680
_diffrn_reflns_av_unetI/netI     0.0743
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            61562
_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         30.508
_diffrn_reflns_theta_min         1.721
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    9.116
_exptl_absorpt_correction_T_max  0.61862
_exptl_absorpt_correction_T_min  0.60956
_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_density_diffrn    2.301
_exptl_crystal_description       sphere
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.023
_exptl_crystal_size_rad          0.037
_refine_diff_density_max         2.726
_refine_diff_density_min         -2.485
_refine_diff_density_rms         0.194
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         17895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0895
_refine_ls_R_factor_gt           0.0503
_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^)+(0.0383P)^2^+5.1403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0999
_refine_ls_wR_factor_ref         0.1160
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11836
_reflns_number_total             17895
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1998064.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4517797--4517805.cif.'
_cod_original_formula_sum        'C31.50 H65.50 Ba2 Br10 N2.50 O14.50 Sb2'
_cod_database_code               4517803
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C12 O6 H24 Ba Sb Br5'
_shelx_estimated_absorpt_t_max   0.818
_shelx_estimated_absorpt_t_min   0.350
_reflns_odcompleteness_completeness 99.98
_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. Uiso/Uaniso restraints and constraints
Uiso(N2A) = Uiso(N2)
Uiso(C28A) = Uiso(C28)
Uiso(C30A) = Uiso(C30) = Uiso(C29) = Uiso(C29A)
Uiso(O14) = Uiso(O14A)
Uiso(O13) = Uiso(O13A)
Uiso(N1A) = Uiso(N1)
Uiso(C26A) = Uiso(C26) = Uiso(C27) = Uiso(C27A)
Uiso(C25) = Uiso(C25A)
3. Others
 Sof(O14A)=Sof(N2A)=Sof(C28A)=Sof(H28A)=Sof(C29A)=Sof(H29D)=Sof(H29E)=
 Sof(H29F)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(O14)=Sof(N2)=Sof(C28)=Sof(H28)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H29C)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Sof(O13A)=Sof(N1A)=Sof(C25A)=Sof(H25A)=Sof(C26A)=Sof(H26D)=Sof(H26E)=
 Sof(H26F)=Sof(C27A)=Sof(H27D)=Sof(H27E)=Sof(H27F)=1-FVAR(2)
 Sof(O13)=Sof(N1)=Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(H26C)=
 Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H27C)=FVAR(2)
 Fixed Sof: O15(0.5) N3(0.5) C31(0.5) H31(0.5) C32(0.5) H32A(0.5) H32B(0.5)
 H32C(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5)
4.a Free rotating group:
 O13(N1,C25,C26,C27), O13A(N1A,C25A,C26A,C27A), O14(N2,C28,C29,C30), O14A(N2A,
 C28A,C29A,C30A), O15(N3,C31,C32,C33)
4.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), 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)
4.c Me refined with riding coordinates:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C26A(H26D,H26E,H26F), C27A(H27D,
 H27E,H27F), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C29A(H29D,H29E,H29F),
 C30A(H30D,H30E,H30F), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C)
4.d Aromatic/amide H refined with riding coordinates:
 C25(H25), C25A(H25A), C28(H28), C28A(H28A), C31(H31)
;
_shelx_res_checksum              40253
_shelx_hkl_checksum              13187
_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 1.634
_oxdiff_exptl_absorpt_empirical_full_min 0.766