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_4517800
_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(Cs), Cl5 Sb, 2(C12 H24 O6), C3 H7 N1 O1'
_chemical_formula_sum            'C27 H55 Cl5 Cs2 N O13 Sb'
_chemical_formula_weight         1166.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 98.4941(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.1006(3)
_cell_length_b                   8.53683(13)
_cell_length_c                   24.3975(4)
_cell_measurement_reflns_used    15557
_cell_measurement_temperature    230.0(2)
_cell_measurement_theta_max      27.3790
_cell_measurement_theta_min      1.9630
_cell_volume                     4346.57(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.23a (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.23a (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.23a (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      230.0(2)
_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    -33.00  -3.00   1.00  125.00    --  -24.99 -38.00 120.00   30
  2  \w    -94.00   4.00   1.00  125.00    --  -24.99 -77.00   0.00   98
  3  \w     -5.00  43.00   1.00  125.00    --  -24.99  57.00   0.00   48
  4  \w    -79.00   4.00   1.00  125.00    --  -24.99 -77.00 120.00   83
  5  \w    -94.00   4.00   1.00  125.00    --  -24.99 -77.00-120.00   98
  6  \w    -71.00 -39.00   1.00  125.00    --  -24.99 -38.00 120.00   32
  7  \w    -45.00  48.00   1.00  125.00    --   25.46 -38.00  90.00   93
  8  \w     28.00  85.00   1.00  125.00    --   25.46-133.00 -92.03   57
  9  \w    -25.00  65.00   1.00  125.00    --   25.46 -99.00 -30.00   90
 10  \w    -38.00  76.00   1.00  125.00    --   25.46   0.00 150.00  114
 11  \w      1.00  85.00   1.00  125.00    --   25.46-132.00 126.04   84
;
_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      0.0339061000
_diffrn_orient_matrix_UB_12      0.0054941000
_diffrn_orient_matrix_UB_13      0.0036547000
_diffrn_orient_matrix_UB_21      -0.0010692000
_diffrn_orient_matrix_UB_22      0.0596823000
_diffrn_orient_matrix_UB_23      0.0200741000
_diffrn_orient_matrix_UB_31      0.0021360000
_diffrn_orient_matrix_UB_32      -0.0575286000
_diffrn_orient_matrix_UB_33      0.0211630000
_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  0.0839
_diffrn_reflns_av_unetI/netI     0.0571
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            83623
_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         29.575
_diffrn_reflns_theta_min         1.821
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.646
_exptl_absorpt_correction_T_max  0.84511
_exptl_absorpt_correction_T_min  0.84360
_exptl_absorpt_correction_type   multi-scan
_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    1.783
_exptl_crystal_description       plate
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.01
_exptl_crystal_size_rad          0.043
_refine_diff_density_max         0.487
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         12187
_refine_ls_number_restraints     616
_refine_ls_restrained_S_all      0.985
_refine_ls_R_factor_all          0.0690
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0147P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0519
_refine_ls_wR_factor_ref         0.0587
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8574
_reflns_number_total             12187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1998078.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 4517797--4517805.cif.'
_cod_database_code               4517800
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C24 O12 H48 Cs2 Sb Cl5'
_shelx_estimated_absorpt_t_max   0.974
_shelx_estimated_absorpt_t_min   0.742
_reflns_odcompleteness_completeness 99.96
_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. Restrained distances
 O12-C22 \\sim O12A-C22A \\sim O12-C23 \\sim O12A-C23A \\sim O7-C24 \\sim
O7A-C24A \\sim O7-C13 \\sim O7A-
 C13A \\sim O8-C25 \\sim O8A-C14A \\sim O8-C26 \\sim O8A-C15A \\sim O9-C27
\\sim O9A-C16A \\sim O9-C17 ~
 O9A-C17A \\sim O10-C18 \\sim O10A-C18A \\sim O11-C20 \\sim O11A-C20A
 with sigma of 0.02
 N1A-C1B \\sim N1-C15 \\sim N1-C16 \\sim N1A-C1A
 with sigma of 0.02
 O13-C14 \\sim O13A-C28
 with sigma of 0.02
 C19-C20 \\sim C19A-C20A \\sim C22A-C21A \\sim C22-C21 \\sim C24A-C23A \\sim
C24-C23 \\sim C25-C13 ~
 C14A-C13A \\sim C16A-C15A \\sim C27-C26 \\sim C18-C17 \\sim C18A-C17A
 with sigma of 0.02
 N1-C14 \\sim N1A-C28
 with sigma of 0.02
3. Rigid bond restraints
 O7, O8, O9, O10, O11, O12, C13, C17, C18, C19, C20, C21, C22, C23, C24, C25,
 C26, C27, O7A, O8A, O9A, O10A, O11A, O12A, C13A, C14A, C15A, C16A, C17A, C18A,
 C19A, C20A, C21A, C22A, C23A, C24A
 with sigma for 1-2 distances of 0.0025 and sigma for 1-3 distances of 0.0025
 O13, O13A, N1, N1A, C1A, H1AA, H1AB, H1AC, C1B, H1BA, H1BB, H1BC, C14, H14,
 C15, H15C, H15D, H15E, C16, H16C, H16D, H16E, C28, H28
 with sigma for 1-2 distances of 0.0025 and sigma for 1-3 distances of 0.0025
4. Uiso/Uaniso restraints and constraints
Uanis(N1) = Uanis(N1A)
Uanis(C1A) = Uanis(C16)
Uanis(C14) = Uanis(C28)
Uanis(C1B) = Uanis(C15)
5. Rigid body (RIGU) restrains
 O7, O8, O9, O10, O11, O12, C13, C17, C18, C19, C20, C21, C22, C23, C24, C25,
 C26, C27, O7A, O8A, O9A, O10A, O11A, O12A, C13A, C14A, C15A, C16A, C17A, C18A,
 C19A, C20A, C21A, C22A, C23A, C24A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O13, O13A, N1, N1A, C1A, H1AA, H1AB, H1AC, C1B, H1BA, H1BB, H1BC, C14, H14,
 C15, H15C, H15D, H15E, C16, H16C, H16D, H16E, C28, H28
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
6. Others
 Sof(O7A)=Sof(O8A)=Sof(O9A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=Sof(C13A)=Sof(H13C)=
 Sof(H13D)=Sof(C14A)=Sof(H14A)=Sof(H14B)=Sof(C15A)=Sof(H15A)=Sof(H15B)=
 Sof(C16A)=Sof(H16A)=Sof(H16B)=Sof(C17A)=Sof(H17C)=Sof(H17D)=Sof(C18A)=
 Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19C)=Sof(H19D)=Sof(C20A)=Sof(H20C)=
 Sof(H20D)=Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C22A)=Sof(H22C)=Sof(H22D)=
 Sof(C23A)=Sof(H23C)=Sof(H23D)=Sof(C24A)=Sof(H24C)=Sof(H24D)=1-FVAR(1)
 Sof(O7)=Sof(O8)=Sof(O9)=Sof(O10)=Sof(O11)=Sof(O12)=Sof(C13)=Sof(H13A)=
 Sof(H13B)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=
 Sof(H19A)=Sof(H19B)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=
 Sof(C22)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=
 Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=
 Sof(H27A)=Sof(H27B)=FVAR(1)
 Sof(O13A)=Sof(N1A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(C1B)=Sof(H1BA)=
 Sof(H1BB)=Sof(H1BC)=Sof(C28)=Sof(H28)=1-FVAR(2)
 Sof(O13)=Sof(N1)=Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15C)=Sof(H15D)=Sof(H15E)=
 Sof(C16)=Sof(H16C)=Sof(H16D)=Sof(H16E)=FVAR(2)
7.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), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
  C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,
 H24B), C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B), C13A(H13C,H13D),
 C14A(H14A,H14B), C15A(H15A,H15B), C16A(H16A,H16B), C17A(H17C,H17D), C18A(H18C,
 H18D), C19A(H19C,H19D), C20A(H20C,H20D), C21A(H21C,H21D), C22A(H22C,H22D),
 C23A(H23C,H23D), C24A(H24C,H24D)
7.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C28(H28)
7.c Idealised Me refined as rotating group:
 C1A(H1AA,H1AB,H1AC), C1B(H1BA,H1BB,H1BC), C15(H15C,H15D,H15E), C16(H16C,H16D,
 H16E)
;
_shelx_res_checksum              89001
_shelx_hkl_checksum              9275
_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 1.239
_oxdiff_exptl_absorpt_empirical_full_min 0.886