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_4517804
_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(K), 2(C12 H24 O6), 2(C3 H7 N O)'
_chemical_formula_sum            'C30 H62 Br5 K2 N2 O14 Sb'
_chemical_formula_weight         1274.31
_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             2020-04-20
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-20 # Formatted by publCIF
;
_cell_angle_alpha                81.641(6)
_cell_angle_beta                 81.407(7)
_cell_angle_gamma                83.885(6)
_cell_formula_units_Z            1
_cell_length_a                   10.3871(8)
_cell_length_b                   10.5079(7)
_cell_length_c                   11.1570(9)
_cell_measurement_reflns_used    4035
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      32.4620
_cell_measurement_theta_min      2.5120
_cell_volume                     1186.80(16)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0839
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.819
_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    -97.00  13.00   1.00   15.00    --  -25.15 -19.00 120.00  110
  2  \w    -44.00  54.00   1.00   15.00    --   25.62 -77.00 120.00   98
  3  \w     -3.00  95.00   1.00   15.00    --   25.62  77.00  60.00   98
  4  \w    -99.00 -34.00   1.00   15.00    --  -25.15-179.00 150.00   65
;
_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      -0.0333453000
_diffrn_orient_matrix_UB_12      -0.0246907000
_diffrn_orient_matrix_UB_13      -0.0414477000
_diffrn_orient_matrix_UB_21      -0.0402034000
_diffrn_orient_matrix_UB_22      -0.0319548000
_diffrn_orient_matrix_UB_23      0.0499047000
_diffrn_orient_matrix_UB_31      -0.0455770000
_diffrn_orient_matrix_UB_32      0.0553030000
_diffrn_orient_matrix_UB_33      -0.0002623000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0580
_diffrn_reflns_Laue_measured_fraction_full 0.948
_diffrn_reflns_Laue_measured_fraction_max 0.819
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11717
_diffrn_reflns_point_group_measured_fraction_full 0.948
_diffrn_reflns_point_group_measured_fraction_max 0.819
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.634
_diffrn_reflns_theta_min         1.966
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    5.022
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26581
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.23a (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.344
_refine_diff_density_min         -1.430
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         7098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0305P)^2^+0.2400P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0866
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5939
_reflns_number_total             7098
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            1998071.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 4517797--4517805.cif.'
_cod_database_code               4517804
_shelx_shelxl_version_number     2017/1
_publcif_funding_html
;

;
_chemical_oxdiff_formula         'C24 H48 O12 K2 Sb Br5'
_shelx_estimated_absorpt_t_max   0.634
_shelx_estimated_absorpt_t_min   0.108
_reflns_odcompleteness_completeness 91.77
_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.a Secondary CH2 refined with riding coordinates:
 C00D(H00A,H00B), C00E(H00C,H00D), C00F(H00E,H00F), C00G(H00G,H00H), C00H(H00I,
 H00J), C00I(H00K,H00L), C00J(H00M,H00N), C00K(H00O,H00P), C00L(H00Q,H00R),
 C00M(H00S,H00T), C00N(H00U,H00V), C00O(H00W,H00X)
2.b Aromatic/amide H refined with riding coordinates:
 C00R(H00Z)
2.c Idealised Me refined as rotating group:
 C00Q(H00Y,H,HA), C00S(H00,HB,HC)
;
_shelx_res_checksum              23292
_shelx_hkl_checksum              65642
_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 2.464
_oxdiff_exptl_absorpt_empirical_full_min 0.577