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_4517799
_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
'Br5 Sb, 2(Rb), 2(C12 H24 O6), 2.001(C3 H7 N O)'
_chemical_formula_sum            'C30 H62 Br5 N2 O14 Rb2 Sb'
_chemical_formula_weight         1367.05
_chemical_name_systematic
'Rubidium pentabromoantimonate(III) 1,4,7,10,13,16-hexaoxacyclooctadecane N,N-dimethylformamide'
_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             2020-05-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                80.574(4)
_cell_angle_beta                 80.343(3)
_cell_angle_gamma                82.145(4)
_cell_formula_units_Z            1
_cell_length_a                   10.5860(4)
_cell_length_b                   10.6601(6)
_cell_length_c                   11.3458(5)
_cell_measurement_reflns_used    9932
_cell_measurement_temperature    250.00(10)
_cell_measurement_theta_max      29.0140
_cell_measurement_theta_min      2.4710
_cell_volume                     1237.29(10)
_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      250.00(10)
_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 0.879
_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    -77.00 -35.00   1.00   28.01    --  -16.74 133.00 -42.70   42
  2  \w    -19.00  21.00   1.00   28.01    --  -16.74 -99.00 120.00   40
  3  \w    -80.00  -5.00   1.00   28.01    --  -16.74 138.00 147.21   75
  4  \w    -86.00  -9.00   1.00   28.01    --  -16.74 -77.00 -30.00   77
  5  \w    -85.00  -6.00   1.00   28.01    --  -16.74 -57.00-150.00   79
  6  \w    -84.00  -9.00   1.00   28.01    --  -16.74 144.00-130.19   75
  7  \w     -4.00  88.00   1.00   28.01    --   17.21  38.00  90.00   92
  8  \w     -5.00  87.00   1.00   28.01    --   17.21  38.00-180.00   92
  9  \w    -48.00  36.00   1.00   28.01    --   17.21 -57.00  90.00   84
 10  \w    -11.00  48.00   1.00   28.01    --   17.21 -19.00 -60.00   59
;
_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      -0.0031692000
_diffrn_orient_matrix_UB_12      -0.0082866000
_diffrn_orient_matrix_UB_13      0.0637059000
_diffrn_orient_matrix_UB_21      0.0152219000
_diffrn_orient_matrix_UB_22      -0.0669873000
_diffrn_orient_matrix_UB_23      0.0007559000
_diffrn_orient_matrix_UB_31      0.0665962000
_diffrn_orient_matrix_UB_32      0.0071216000
_diffrn_orient_matrix_UB_33      -0.0069275000
_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  0.0290
_diffrn_reflns_av_unetI/netI     0.0283
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19733
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.295
_diffrn_reflns_theta_min         1.840
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    6.603
_exptl_absorpt_correction_T_max  0.93985
_exptl_absorpt_correction_T_min  0.93985
_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    1.835
_exptl_crystal_description       block
_exptl_crystal_F_000             668
_exptl_crystal_recrystallization_method 'from N,N-dimethylformamide'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_crystal_size_rad          0.1
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.827
_refine_diff_density_rms         0.079
_refine_ls_extinction_coef       0.0151(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         5954
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0278
_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^)+(0.0299P)^2^+1.0835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0657
_refine_ls_wR_factor_ref         0.0690
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5106
_reflns_number_total             5954
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1997957.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4517797--4517805.cif.'
_cod_database_code               4517799
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Cs2 C24 H48 O12 Sb Br5'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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(C13C) = Uiso(C13B) = Uiso(C13)
Uiso(C15B) = Uiso(C15C) = Uiso(C14) = Uiso(C15) = Uiso(C14B) = Uiso(C14C)
Uiso(N1C) = Uiso(N1B) = Uiso(N1)
Uiso(O7B) = Uiso(O7C) = Uiso(O7)
3. Others
 1*[Sof(O7B)+Sof(N1B)+Sof(C13B)+Sof(H13B)+Sof(C14B)+Sof(H14D)+Sof(H14E)+
 Sof(H14F)+Sof(C15B)+Sof(H15D)+Sof(H15E)+Sof(H15F)]+1*[Sof(O7)+Sof(N1)+Sof(C13)+
 Sof(H13)+Sof(C14)+Sof(H14A)+Sof(H14B)+Sof(H14C)+Sof(C15)+Sof(H15A)+Sof(H15B)+
 Sof(H15C)]+1*[Sof(O7C)+Sof(N1C)+Sof(C13C)+Sof(H13C)+Sof(C14C)+Sof(H14G)+
 Sof(H14H)+Sof(H14I)+Sof(C15C)+Sof(H15G)+Sof(H15H)+Sof(H15I)]=1 with esd of
 0.001
 Sof(O7B)=Sof(N1B)=Sof(C13B)=Sof(H13B)=Sof(C14B)=Sof(H14D)=Sof(H14E)=Sof(H14F)=
 Sof(C15B)=Sof(H15D)=Sof(H15E)=Sof(H15F)=FVAR(1)
 Sof(O7)=Sof(N1)=Sof(C13)=Sof(H13)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=
 Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=FVAR(2)
 Sof(O7C)=Sof(N1C)=Sof(C13C)=Sof(H13C)=Sof(C14C)=Sof(H14G)=Sof(H14H)=Sof(H14I)=
 Sof(C15C)=Sof(H15G)=Sof(H15H)=Sof(H15I)=FVAR(3)
 Fixed Sof: Br1(0.5)
4.a Free rotating group:
 O7(N1,C13,C14,C15), O7B(N1B,C13B,C14B,C15B), O7C(N1C,C13C,C14C,C15C)
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)
4.c Me refined with riding coordinates:
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C14B(H14D,H14E,H14F), C15B(H15D,
 H15E,H15F), C14C(H14G,H14H,H14I), C15C(H15G,H15H,H15I)
4.d Aromatic/amide H refined with riding coordinates:
 C13(H13), C13B(H13B), C13C(H13C)
;
_shelx_res_checksum              61391
_shelx_hkl_checksum              31912
_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 1.530
_oxdiff_exptl_absorpt_empirical_full_min 0.817